CN106588021B - 一种碳化硅陶瓷及其制备方法 - Google Patents
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Abstract
本发明提供了一种碳化硅陶瓷及其制备方法。所述方法包括以如下重量百分比成分为原料经过冷等静压和液相烧结进行制备:陶瓷主原料、占陶瓷主原料重量2.5%‑3.5%的粘结剂和占陶瓷主原料重量1.5%‑2.5%的分散剂。一般的陶瓷材料成型都采用干压成型,干压成型时,由于压力分布不均匀而造成坯体内部密度分布不一致,从而影响材料的各种性能;相比较干压成型,冷等静压成型施压均匀,材料各个方向受到的压力相同,使材料的烧结密度、弯曲强度、抗折强度得到提高。
Description
技术领域
本发明涉及陶瓷加工领域,具体的说,涉及一种碳化硅陶瓷及其制备方法。
背景技术
碳化硅(SiC)是典型的共价键化合物,单位晶胞由相同的硅碳四面体构成,硅原子处于中心,周围是碳。SiC晶体结构中C和Si键长,共价性强,晶格缺陷小,这种共价键合特征使碳化硅陶瓷材料具有优异的高温强度、耐磨性、耐腐蚀性及良好的导电、导热性;在航空、航天、机械、汽车、石化、冶金和电子等行业得到广泛应用。
目前碳化硅陶瓷作为内加热器保护套管在热浸镀锌领域已经得到了一定的应用,但单质的传统碳化硅制品不耐冲击,抗锌渣锌灰缠绕结瘤能力差,抗冲击性能差,不能随炉冷却,因此在国内使用时并未取得良好的经济效果。碳化硅基复合材料可以提高碳化硅材料的抗冲击性能,抗热震性能等,较单质碳化硅材料更优,更适宜于充当内加热器保护套材料。因此,需要寻找合理的配方与烧结制度来制得满足热浸镀锌使用工况的碳化硅基陶瓷材料。
发明内容
本发明的一个目的在于提供一种碳化硅陶瓷;该碳化硅陶瓷不仅具有较高的抗折强度、导热率和耐锌液侵蚀性能,而且还具有耐热震性和可加工性能。
本发明的另一目的在于提供所述碳化硅陶瓷的制备方法。
为达上述目的,一方面,本发明提供了一种碳化硅陶瓷的制备方法,其中,所述方法包括以如下重量百分比成分为原料经过冷等静压和液相烧结进行制备:陶瓷主原料、占陶瓷主原料重量2.5%-3.5%的粘结剂和占陶瓷主原料重量1.5%-2.5%的分散剂。
根据本发明一些具体实施方案,其中,所述陶瓷主原料以陶瓷主原料总重量为100%计包括如下重量百分比成分:碳化硅60%-70%、氮化硼或鳞片石墨8%-13%、硅粉5%-10%、氧化铝6%和三氧化二钇4%。
根据本发明一些具体实施方案,其中,本发明是在惰性气体中液相烧结得到碳化硅陶瓷。
其中氮化硼或鳞片石墨作为与陶瓷基体形成弱结合界面的第二相,不仅提高了碳化硅陶瓷的可加工性能,对陶瓷材料抗热震性能的提高也有积极的作用。
氮化硼或鳞片石墨与碳化硅体系之间难以烧结,所以引入氮化硼或鳞片石墨后材料的抗折强度有显著下降,为了在能够保持材料具有较高的热导率的条件下解决该问题,本发明发现硅粉能够增加碳化硅体系的强度。硅粉的作用有两个:
1.硅粉会与保护气氛氮气发生反应生成氮化硅。
2.硅粉能够在不同体系的试样中对细小的空隙进行填充。
根据本发明一些具体实施方案,其中,所述氮化硼为六方氮化硼。
根据本发明一些具体实施方案,其中,所述粘结剂选自聚乙烯醇;
根据本发明一些具体实施方案,其中,所述分散剂选自四甲基氢氧化铵。
根据本发明一些具体实施方案,其中,所述碳化硅为按照如下粒径比配制的粉末:200μm:60μm:15μm:1μm=0.55:0.2:0.2:0.05。
对于采购的工业级SiC粉料,如何选取颗粒级配是配料工序中最基本的问题。合理的颗粒级配可以降低试样的气孔率,增大试样密度,防止碳化硅发生氧化而导致的各项性能(抗折强度、使用寿命、抗氧化性能等)降低。根据Andreasen基于连续尺寸分布颗粒的堆积理论计算,并根据试验结果调整配比得出上述配比。
根据本发明一些具体实施方案,其中,所述冷等静压是在压力为220-280MPA,保压时间3-8min的条件下对原料进行压坯得到坯体。
根据本发明一些具体实施方案,其中,所述液相烧结是将坯体在1700~1850℃℃,保温时间2-3h的条件下进行烧结。
根据本发明一些具体实施方案,其中,所述原料在经过冷等静压制备坯体后,先将坯体在150~250℃下烘干3~4h,然后在惰性气体中以8~10℃/h的速度升温至1700~1850℃,然后再将坯体进行液相烧结。
根据本发明一些具体实施方案,其中,所述惰性气体为氮气。
根据本发明一些具体实施方案,其中,所述方法具体包括如下步骤:
(1)将所述原料与水混合,配制成固相质量含量为35%-55%的浆料,然后造粉粒;
(2)将造粉粒放入冷等静压模具中,在压力220-280MPa,保压时间3-8min条件下进行压坯得到坯体;
(3)将坯体在150~250℃下烘干3~4h;
(4)然后将坯体在惰性气体中以8~10℃/h的速度升温至1700~1850℃,再保温时间2-3h,然后自然冷却至室温,得到所述碳化硅陶瓷。
根据本发明一些具体实施方案,其中,步骤(1)是将所述原料与水进行球磨混合。
根据本发明一些具体实施方案,其中,步骤(1)中所述水为去离子水。
根据本发明一些具体实施方案,其中,步骤(1)是采用喷雾造粒法造粉粒。
另一方面,本发明还提供了所述制备方法制备得到的碳化硅陶瓷。
综上所述,本发明提供了一种碳化硅陶瓷及其制备方法。本发明的方案具有如下优点:
1)、六方氮化硼(h-BN)具有良好的热稳定性、低的热膨胀系数和优良的抗热震性,将h-BN引入到碳化硅基陶瓷材料,一方面由于h-BN具有像石墨一样的层状结构,层间结合力弱,易于层间剥离,使碳化硅基陶瓷具有良好的可加工性能;另一方面,由于,在陶瓷完成烧结冷却到室温后,陶瓷晶粒之间出现由于SiC和h-BN的热膨胀系数和弹性模量不同而导致的微裂纹,这些微裂纹在陶瓷材料受到张应力时,会分散主裂纹尖端能量,提高了陶瓷的断裂能,从而使碳化硅基陶瓷具有优良的抗热震性能。
2)、碳化硅(SiC)是典型的强共价键化合物,在高温下的自扩散系数相当低,导致其固相烧结在很高的温度下都难以实现,本发明同时将(Si)硅粉和(Al2O3)三氧化二铝/(Y2O3)三氧化二钇碳化硅基陶瓷材料。硅粉作为烧结助剂可显著提高碳化硅的烧结动力学,提高碳化硅陶瓷的烧结强度;Al2O3/Y2O3在高温下形成共熔液相,使体系的传质方式由扩散传质变为粘性流动,降低了陶瓷致密化所需能量和烧结温度,此外,由于Al2O3/Y2O3在高温下形成共熔液相YAG冷却后分布在SiC晶界,YAG中存在许多由于与陶瓷基体热膨胀系数不同而导致的微裂纹,提高陶瓷的抗折强度。
3)、一般的陶瓷材料成型都采用干压成型,干压成型时,由于压力分布不均匀而造成坯体内部密度分布不一致,从而影响材料的各种性能;相比较干压成型,冷等静压成型施压均匀,材料各个方向受到的压力相同,使材料的烧结密度、弯曲强度、抗折强度得到提高。
具体实施方式
以下通过具体实施例详细说明本发明的实施过程和产生的有益效果,旨在帮助阅读者更好地理解本发明的实质和特点,不作为对本案可实施范围的限定。
实施例1
实施方式中的份代表重量份。
碳化硅选用碳化硅粉末(纯度>98%,粒径分别为50μm和10μm),氮化硼选用六方氮化硼颗粒(h-BN,平均粒径小于4μm,纯度>98%)。
步骤1,碳化硅粉末的级配
按质量比200μm:60μm:15μm:1μm=0.55:0.2:0.2:0.05分别称取碳化硅粉末。
步骤2,湿法球磨
将68份碳化硅、12份氮化硼、10份硅粉、6份三氧化二铝和4份三氧化二钇混合,形成主原料;然后加入3份聚乙烯醇、2份四甲基氢氧化铵和120份去离子水,球磨4小时后配置成固相含量为50%的浆料。
步骤3,喷雾造粒
对浆料进行喷雾造粒,工艺条件如下:浆料流量为150ml/min,进口温度为180℃,出口温度为110℃。
步骤4,压坯
将步骤3得到的造粉粒装入冷等静压模具中,密封后采用冷等静压机压制坯料,在压力为220-280MPa,保压时间为3-8min的条件下进行压坯。
步骤5,预烧
将步骤4得到的坯体放入烘箱,在150℃下烘干3小时。
步骤6,烧结
将步骤5预烧后的坯体在氮气中以每小时10℃的升温速率升温到1850℃进行无压液相烧结,保温时间为2小时,使粘结剂分解,随炉自然冷却到室温后,完成烧结,得到耐腐蚀、耐热震和可加工性能的碳化硅陶瓷材料。所述陶瓷材料的抗折强度为60MPa,耐锌液侵蚀速率为0.4mm/a,从600℃到室温,热震30次,无表观裂纹。
实施例2
实施方式中的份代表重量份。
碳化硅选用碳化硅粉末(纯度>98%,粒径分别为50μm和10μm),氮化硼选用六方氮化硼颗粒(h-BN,平均粒径小于4μm,纯度>98%)。
步骤1,碳化硅粉末的级配
按质量比200μm:60μm:15μm:1μm=0.55:0.2:0.2:0.05分别称取碳化硅粉末。
步骤2,湿法球磨
将68份碳化硅、12份氮化硼、10份硅粉、6份三氧化二铝和4份三氧化二钇混合,形成主原料;然后加入3份聚乙烯醇、2份四甲基氢氧化铵和120份去离子水,球磨4小时后配置成固相含量为50%的浆料。
步骤3,喷雾造粒
对浆料进行喷雾造粒,工艺条件如下:浆料流量为150ml/min,进口温度为180℃,出口温度为110℃。
步骤4,压坯
将步骤3得到的造粉粒装入冷等静压模具中,密封后采用冷等静压机压制坯料,在压力为220-280MPa,保压时间为3-8min的条件下进行压坯。
步骤5,预烧
将步骤4得到的坯体放入烘箱,在150℃下烘干3小时。
步骤6,烧结
将步骤5预烧后的坯体在氮气中以每小时8℃的升温速率升温到1700℃进行无压液相烧结,保温时间为3小时,使粘结剂分解,随炉自然冷却到室温后,完成烧结,得到耐腐蚀、耐热震和可加工性能的碳化硅陶瓷材料。所述陶瓷材料的抗折强度不低于55MPa,耐锌液侵蚀速率低于0.5mm/a,从600℃到室温,热震30次,无表观裂纹。
实施例3
实施方式中的份代表重量份。
碳化硅选用碳化硅粉末(纯度>98%,粒径分别为50μm和10μm),氮化硼选用六方氮化硼颗粒(h-BN,平均粒径小于4μm,纯度>98%)。
步骤1,碳化硅粉末的级配
按质量比200μm:60μm:15μm:1μm=0.55:0.2:0.2:0.05分别称取碳化硅粉末。
步骤2,湿法球磨
将68份碳化硅、12份氮化硼、10份硅粉、6份三氧化二铝和4份三氧化二钇混合,形成主原料;然后加入3份聚乙烯醇、2份四甲基氢氧化铵和120份去离子水,球磨4小时后配置成固相含量为50%的浆料。
步骤3,喷雾造粒
对浆料进行喷雾造粒,工艺条件如下:浆料流量为150ml/min,进口温度为180℃,出口温度为110℃。
步骤4,压坯
将步骤3得到的造粉粒装入冷等静压模具中,密封后采用冷等静压机压制坯料,在压力为220-280MPa,保压时间为3-8min的条件下进行压坯。
步骤5,预烧
将步骤4得到的坯体放入烘箱,在150℃下烘干3小时。
步骤6,烧结
将步骤5预烧后的坯体在氮气中以每小时10℃的升温速率升温到1800℃进行无压液相烧结,保温时间为3小时,使粘结剂分解,随炉自然冷却到室温后,完成烧结,得到耐腐蚀、耐热震和可加工性能的碳化硅陶瓷材料。所述陶瓷材料的抗折强度不低于60MPa,耐锌液侵蚀速率为0.45mm/a,从600℃到室温,热震30次,无表观裂纹。
Claims (9)
1.一种碳化硅陶瓷的制备方法,其中,所述方法包括以如下重量百分比成分为原料经过冷等静压和液相烧结进行制备:陶瓷主原料、占陶瓷主原料重量2.5%-3.5%的粘结剂和占陶瓷主原料重量1.5%-2.5%的分散剂;所述陶瓷主原料以陶瓷主原料总重量为100%计包括如下重量百分比成分:碳化硅60%-70%、氮化硼或鳞片石墨8%-13%、硅粉5%-10%、三氧化二铝6%和三氧化二钇4%;所述粘结剂选自聚乙烯醇;所述分散剂选自四甲基氢氧化铵;所述碳化硅陶瓷的抗折强度最高达到70MPa,耐锌液侵蚀速率最低达到0.4mm/a,所述述碳化硅陶瓷从600℃到室温,热震30次,无表观裂纹;所述方法具体包括如下步骤:
(1)将所述原料与水混合,配制成固相质量含量为35%-55%的浆料,然后造粉粒;
(2)将造粉粒放入冷等静压模具中,在压力220-280MPa,保压时间3-8min条件下进行压坯得到坯体;
(3)将坯体在150~250℃下烘干3~4h;
(4)然后将坯体在惰性气体中以8~10℃/h的速度升温至1700~1850℃,再保温时间2-3h,然后自然冷却至室温,得到所述碳化硅陶瓷。
2.根据权利要求1所述的制备方法,其中,所述氮化硼为六方氮化硼。
3.根据权利要求1所述的制备方法,其中,所述碳化硅为按照如下粒径比配制的粉末:200μm:60μm:15μm:1μm=0.55:0.2:0.2:0.05。
4.根据权利要求1所述的制备方法,其中,所述原料在经过冷等静压制备坯体后,先将坯体在150~250℃下烘干3~4h,然后在惰性气体中以8~10℃/h的速度升温至1700~1850℃,进行液相烧结。
5.根据权利要求4所述的制备方法,其中,所述惰性气体为氮气。
6.根据权利要求1所述的制备方法,其中,步骤(1)包括将所述原料与水进行球磨混合。
7.根据权利要求1所述的制备方法,其中,步骤(1)所述水为去离子水。
8.根据权利要求1所述的制备方法,其中,步骤(1)采用喷雾造粒法造粉粒。
9.权利要求1~8任意一项所述制备方法制备得到的碳化硅陶瓷。
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