CN113929471A - 一种耐高温氧化Si3N4/O’-sialon复合陶瓷及其制备方法 - Google Patents

一种耐高温氧化Si3N4/O’-sialon复合陶瓷及其制备方法 Download PDF

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CN113929471A
CN113929471A CN202111314190.0A CN202111314190A CN113929471A CN 113929471 A CN113929471 A CN 113929471A CN 202111314190 A CN202111314190 A CN 202111314190A CN 113929471 A CN113929471 A CN 113929471A
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鲍崇高
马海强
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Xian Jiaotong University
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Abstract

一种耐高温氧化Si3N4/O’‑sialon复合陶瓷及其制备方法，复合陶瓷按照质量百分数计包括如下组分：α‑Si3N4粉体：50wt.％～75wt.％；β‑Si3N4粉体：10wt％～25wt％；SiO2粉体：5wt％～15wt％；Al2O3‑R2O3：8wt％～12wt％；制备方法是将α‑Si3N4、β‑Si3N4、SiO2和Al2O3‑R2O3配成混合粉体，加入无水乙醇进行球磨；再将球磨完的浆料进行干燥获得粉体，之后过筛和成型；最后将成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结；本发明采用添加SiO2原位合成O’‑sialon陶瓷，具有制备方法简单、热力学性能稳定、结合强度和抗氧化性能优异等特点。

Description

一种耐高温氧化Si3N4/O’-sialon复合陶瓷及其制备方法
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种耐高温氧化Si3N4/O’-sialon复合陶瓷及其制备方法。
背景技术
氮化硅作为一类非氧化性陶瓷，在高温-空气环境下易于氧化，导致其性能下降。因此，为了促使氮化硅陶瓷能够更加广泛地应用于实际高温工程领域，提高氮化硅陶瓷的高温氧化性能有着非常重要的意义。
目前，提高氮化硅高温氧化性能的方法可以归纳为以下几类：(1)抗氧化涂层的制备。此种方法主要是在氮化硅陶瓷表面涂覆一层抗氧化涂层，从而保护氮化硅基体；(2)氮化硅复相陶瓷的制备。该方法主要是在氮化硅陶瓷中引入第二相抗氧化性的陶瓷，如MoSi2、TiN和SiC等；(3)氮化硅后处理。该方法主要是将烧结后氮化硅陶瓷进行二次烧结，促使晶界上的非晶态玻璃相晶化；(4)不同稀土氧化物制备氮化硅陶瓷；(5)Si2N2O陶瓷的制备。尽管这些方法提高了氮化硅陶瓷抗氧化性能，但其存在制备过程复杂、热力学不稳定、界面结合强度低和抗氧化性能差等缺点。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种耐高温氧化Si3N4/O’-sialon复合陶瓷及其制备方法，采用添加SiO2原位合成O’-sialon陶瓷，具有制备方法简单、热力学性能稳定、结合强度和抗氧化性能优异等特点。
为了达到上述目的，本发明所采用的技术方案是：
一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：50wt.％～75wt.％；
β-Si3N4粉体：10wt％～25wt％；
SiO2粉体：5wt％～15wt％；
Al2O3-R2O3：8wt％～12wt％。
所述的α-Si3N4粉体的粒径范围为0.4μm～1μm；
所述的β-Si3N4粉体的粒径范围为1μm～2μm；
所述的SiO2粉体的粒径范围为1μm～10μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为Y2O3、Yb2O3或La2O3中的一种，其中Al2O3的质量百分数含量为2wt％～4wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％～8wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨5h～15h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为5℃/min～10℃/min，烧结温度为1750℃～1850℃，保温时间为2h～3h，氮气压力为3MPa～5MPa。
所述的步骤2)中干燥方式为真空干燥或旋转蒸发仪干燥。
所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa～200MPa。
本发明的有益效果在于：
(1)本发明Si3N4/O’-sialon复合陶瓷制备方法简单、热力学性能稳定和抗氧化性能优异，在高温-空气的环境下使用可以形成一层致密的抗氧化保护层。
(2)本发明添加SiO2可以提高氮化硅陶瓷的抗氧化性能，SiO2可以与Si3N4和Al2O3原位形成O’-sialon陶瓷，所形成的O’-sialon位于晶界上，可以有效阻碍空气中的氧从外向内扩散及金属阳离子从内向外扩散，提高了氮化硅陶瓷的抗氧化性能。
附图说明
图1为发明实施例5所得样品的XRD图谱。
图2为发明实施例5所得样品在1500℃空气氧化30h后的微观组织形貌。
具体实施方式
下面结合实施例对本发明做详细描述。
实施例1，一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：50wt.％；
β-Si3N4粉体：25wt％；
SiO2粉体：15wt％；
Al2O3-R2O3：10wt％；
所述的α-Si3N4粉体的粒径范围为0.4μm；
所述的β-Si3N4粉体的粒径范围为1μm；
所述的SiO2粉体的粒径范围为1μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为Y2O3，其中Al2O3的质量百分数含量为2wt％，R2O3(稀土氧化物)的质量百分数含量为8wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨5h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为5℃/min，烧结温度为1750℃，保温时间为2h，氮气压力为3MPa；
所述的步骤2)中干燥方式为真空干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa。
本实施例的有益效果为：本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷1500℃空气氧化30h后氧化增重为0.96mg.cm-2，残余弯曲强度为142.36MPa。
实施例2，一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：75wt.％；
β-Si3N4粉体：10wt％；
SiO2粉体：5wt％；
Al2O3-R2O3：10wt％；
所述的α-Si3N4粉体的粒径范围为1μm；
所述的β-Si3N4粉体的粒径范围为2μm；
所述的SiO2粉体的粒径范围为10μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为Yb2O3，其中Al2O3的质量百分数含量为4wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨15h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为10℃/min，烧结温度为1850℃，保温时间为3h，氮气压力为5MPa；
所述的步骤2)中干燥方式为旋转蒸发仪干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为200MPa。
本实施例的有益效果为：本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷1500℃空气氧化30h后氧化增重为0.92mg.cm-2，残余弯曲强度为189.54MPa。
实施例3，一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：52wt.％；
β-Si3N4粉体：25wt％；
SiO2粉体：15wt％；
Al2O3-R2O3：8wt％；
所述的α-Si3N4粉体的粒径范围为0.5μm；
所述的β-Si3N4粉体的粒径范围为1.5μm；
所述的SiO2粉体的粒径范围为5μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为La2O3，其中Al2O3的质量百分数含量为2wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨14h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为8℃/min，烧结温度为1780℃，保温时间为2.5h，氮气压力为4MPa；
所述的步骤2)中干燥方式为真空干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为100MPa。
本实施例的有益效果为：本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷1500℃空气氧化30h后氧化增重为1.12mg.cm-2，残余弯曲强度为154.29MPa。
实施例4，一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：68wt.％；
β-Si3N4粉体：10wt％；
SiO2粉体：10wt％；
Al2O3-R2O3：12wt％；
所述的α-Si3N4粉体的粒径范围为0.5μm；
所述的β-Si3N4粉体的粒径范围为1.5μm；
所述的SiO2粉体的粒径范围为5μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为La2O3，其中Al2O3的质量百分数含量为4wt％，R2O3(稀土氧化物)的质量百分数含量为8wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨14h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为8℃/min，烧结温度为1780℃，保温时间为2.5h，氮气压力为4MPa；
所述的步骤2)中干燥方式为真空干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa。
本实施例的有益效果为：本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷1500℃空气氧化30h后氧化增重为0.78mg.cm-2；残余弯曲强度为178.65MPa。
实施例5，一种耐高温氧化Si3N4/O’-sialon复合陶瓷，按照质量百分数计包括如下组分：
α-Si3N4粉体：57.5wt.％；
β-Si3N4粉体：20wt％；
SiO2粉体：12.5wt％；
Al2O3-R2O3：10wt％；
所述的α-Si3N4粉体的粒径范围为0.5μm；
所述的β-Si3N4粉体的粒径范围为1.5μm；
所述的SiO2粉体的粒径范围为5μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为Y2O3，其中Al2O3的质量百分数含量为4wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％。
一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨14h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为10℃/min，烧结温度为1750℃，保温时间为2h，氮气压力为3MPa；
所述的步骤2)中干燥方式为真空干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa。
本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷进行X射线衍射分析，结果见图1，材料按预期合成了O’-sialon相，具有热力学性能稳定、结合强度和抗氧化性能；此外，本实施例获得的Si3N4/O’-sialon复合陶瓷在1500℃空气氧化30h后的微观组织如图2所示，由图2可见，得到的Si3N4/O’-sialon复合陶瓷经过高温氧化后表面形成致密的氧化层，阻碍了空气由外向内扩散，提高了材料的抗氧化性能。
本实施例耐高温氧化Si3N4/O’-sialon复合陶瓷1500℃空气氧化30h后氧化增重为0.85mg.cm-2，残余弯曲强度为165.23MPa。
对比例：其制备方法与实施例5大致相同，不同之处在于步骤1中不加SiO2。测试结果得出本对比例所得的复合陶瓷在1500℃空气氧化30h后氧化增重为2.02mg.cm-2，残余弯曲强度为124.36MPa。
实施例1耐高温氧化Si3N4/O’-sialon复合陶瓷相比较于对比例复合陶瓷氧化增重降低了52.47％，残余弯曲强度增加了14.47％。实施例2耐高温氧化Si3N4/O’-sialon复合陶瓷相比较于对比例复合陶瓷氧化增重降低了54.45％和残余弯曲强度增加了52.41％。实施例3耐高温氧化Si3N4/O’-sialon复合陶瓷相比较于对比例复合陶瓷氧化增重降低了44.55％和残余弯曲强度增加了24.07％。实施例4耐高温氧化Si3N4/O’-sialon复合陶瓷相比较于对比例复合陶瓷氧化增重降低了61.39％和残余弯曲强度增加了43.66％。实施例5耐高温氧化Si3N4/O’-sialon复合陶瓷相比较于对比例复合陶瓷氧化增重降低了57.92％和残余弯曲强度增加了32.86％。

Claims (8)

1.一种耐高温氧化Si3N4/O’-sialon复合陶瓷，其特征在于，按照质量百分数计包括如下组分：
α-Si3N4粉体：50wt.％～75wt.％；
β-Si3N4粉体：10wt％～25wt％；
SiO2粉体：5wt％～15wt％；
Al2O3-R2O3：8wt％～12wt％。
2.根据权利要求1所述的一种耐高温氧化Si3N4/O’-sialon复合陶瓷，其特征在于：所述的α-Si3N4粉体的粒径范围为0.4μm～1μm；
所述的β-Si3N4粉体的粒径范围为1μm～2μm；
所述的SiO2粉体的粒径范围为1μm～10μm。
3.根据权利要求1所述的一种耐高温氧化Si3N4/O’-sialon复合陶瓷，其特征在于：所述的Al2O3-R2O3中R2O3(稀土氧化物)为Y2O3、Yb2O3或La2O3中的一种，其中Al2O3的质量百分数含量为2wt％～4wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％～8wt％。
4.权利要求1所述的一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，其特征在于，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨5h～15h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为5℃/min～10℃/min，烧结温度为1750℃～1850℃，保温时间为2h～3h，氮气压力为3MPa～5MPa。
5.根据权利要求4所述的方法，其特征在于：所述的步骤2)中干燥方式为真空干燥或旋转蒸发仪干燥。
6.根据权利要求4所述的方法，其特征在于：所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa～200MPa。
7.一种耐高温氧化Si3N4/O’-sialon复合陶瓷，其特征在于，按照质量百分数计包括如下组分：
α-Si3N4粉体：57.5wt.％；
β-Si3N4粉体：20wt％；
SiO2粉体：12.5wt％；
Al2O3-R2O3：10wt％；
所述的α-Si3N4粉体的粒径范围为0.5μm；
所述的β-Si3N4粉体的粒径范围为1.5μm；
所述的SiO2粉体的粒径范围为5μm；
所述的Al2O3-R2O3中R2O3(稀土氧化物)为Y2O3，其中Al2O3的质量百分数含量为4wt％，R2O3(稀土氧化物)的质量百分数含量为6wt％。
8.权利要求7所述的一种耐高温氧化Si3N4/O’-sialon复合陶瓷的制备方法，其特征在于，按照如下步骤进行：
1)按照质量比称取α-Si3N4、β-Si3N4、SiO2和Al2O3-R2O3配成混合粉体，加入占混合粉体质量40％的无水乙醇进行球磨14h；
2)将球磨完的浆料进行干燥获得粉体，之后过筛和成型；
3)将步骤2)中成型的坯体置于气压烧结炉中，采用氮气作为保护气体进行烧结，升温速率为10℃/min，烧结温度为1750℃，保温时间为2h，氮气压力为3MPa；
所述的步骤2)中干燥方式为真空干燥；
所述的步骤2)中成型方式是模压成型，模压成型的压力为80MPa。
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