CN106278284A - 一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法 - Google Patents

一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法 Download PDF

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CN106278284A
CN106278284A CN201610642334.8A CN201610642334A CN106278284A CN 106278284 A CN106278284 A CN 106278284A CN 201610642334 A CN201610642334 A CN 201610642334A CN 106278284 A CN106278284 A CN 106278284A
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boron nitride
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钱建军
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CHANGXIN XINYU REFRACTORY Co Ltd
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Abstract

本发明涉及一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，属于绝缘材料制备领域。氮化硼制备过程是先将BN基粉体与添加剂和助烧剂混合造粒；然后将混合后的粉末装入环形石墨模具中，进行分步热压烧结；烧结后得到氮化硼陶瓷材料。该方法中，分步热压烧结的工艺包括低温真空保持步骤，中温氮气保压步骤以及高温惰性气氛保压步骤；通过该工艺，可以有效促进气体杂质排出，提高氮化硼陶瓷材料的致密度与强度。

Description

一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法
技术领域
本发明一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，属于绝缘材料制备领域。
背景技术
氮化硼俗称白石墨，特性与石墨相似而质地洁白，存在两种晶型：六方与立方，通常呈六方结构。在高温与超高压的特殊条件下，六方结构晶型可转化为立方晶型。其中六方氮化硼使用范围广泛，其粉末可作为优良的润滑剂与脱模剂，而陶瓷可用作熔炼蒸发金属的坩埚、舟皿、液态金属输送管、火箭喷口，大功率器件底座，半导体元件掺杂源，以及各种高温（高压、高频）绝缘散热部件。
目前六方氮化硼的制备方法包括冷压法与热压法，其中热压法制备的陶瓷密度高、强度高，生产工艺成熟等优点得到广泛应用。如103626498A公开了一种氮化硼陶瓷喷嘴，在氮化硼中加入碳化硅、氧化锆以及其他添加剂，从而提高氮化硼陶瓷的使用寿命；103922773A公开了一种薄带连铸用氮化硼质陶瓷，在六方氮化硼中加入氮化铝粉末，镁铝尖晶石，莫来石等其他添加剂，来提高氮化硼陶瓷的抗热震性以及降低热导率；104193341A公开了一种六方氮化硼陶瓷的制备方法，先采用冷压成型，然后在空气气氛下以及氮气气氛下进行无压烧结来制备，从而提高氮化硼陶瓷的导热性，降低生产成本。
常规的氮化硼制备方法中，采用石墨模具进行坯体成型，由于涉及到压力和温度较高，石墨模具容易发生开裂等问题，严重影响材料的制备效率。
发明内容
本发明通过提供一种氮化硼的新型石墨成型模具，以提高氮化硼陶瓷材料的制备效率。
一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，该方法包括以下步骤：
（1）将含有添加剂和祝烧剂的BN基粉体混合造粒；
（2）将混合后的粉末装入环形石墨模具中，进行分步热压烧结；
（3）烧结后得到氮化硼陶瓷材料；
该发明中，环形石墨模具包括内环与外环，内环与外环之间缝隙为5~20mm。
优选的，热压烧结的工艺包括低温保持步骤，中温保压步骤以及高温保压步骤；低温保持步骤为500~800℃，保温时间为0.5~2小时；中温保压步骤为1000~1500℃，压力15~20MPa，保压时间为0.5~2小时；高温保压步骤为1600~1900℃，压力16~25MPa，保压时间为1~3小时；
该方法中，低温在真空下进行，中温在氮气气氛下进行，高温在惰性气氛下进行。
该方法中，优选的添加剂包括CaO、SiC、Si3N4、ZrO2、 Al2O3 、Y2O3中的一种或多种，助烧剂包括B2O3。
更加优选的，添加剂含量为15~30wt.%，助烧剂含量为5~10wt.%，余量为BN粉体。
本发明的重点在于多步保压工艺，其中在低温阶段，在真空气氛下，易挥发的气体排出，在中温阶段，通过加热，有利于难挥发的气体杂质排出，从而保证了最终氮化硼陶瓷材料的纯度、致密度与强度。
本发明中的成分，除了主成分BN外，还包括一定量的添加剂与助烧剂。
其中助烧剂有利于烧结过程中的粉体间结合。
添加剂中，氧化钇是最优秀的陶瓷材料稳定剂，氧化钇与材质中的氮化硼、氧化锆以及碳化硅都具有十分稳定的亲和力，氧化钇掺入使得本发明陶瓷材料更加具有优良的抗热震性能，提高材质的抗弯强度和断裂韧性。
Al2O3具有很强的粘结力和耐散裂性，Al2O3在高温下形成的液相能够有效地粘结BN。Al2O3与 SiC 表面的氧化物在高温下反应形成硅铝酸盐液相，促进 SiC 陶瓷的烧结致密化。在高温下，Al2O3与ZrO2能产生共融现象，提高烧结密度的均匀性。SiC与Si3N4均有利于强度的提高。
本发明中，石墨模具为环形，环形模具相对于方形模具，各方向上受力均匀。石墨外环与外环之间存在一定的间隙，使内环在高温膨胀基础上，保证内外环之间的接触紧密，从而避免了石墨模具的开裂问题，有利于生产效率的提高。
附图说明
图1氮化硼的热压烧结示意图，其中1为上压头，2为石墨模具，3为下压头，4为最终成型的氮化硼陶瓷坯体。
图2为石墨模具示意图。
具体实施方式
下面结合实施例对本发明做进一步的描述。
实施例 1
准备氮化硼基粉体，其中添加剂为SiC，含量为20wt.%，助烧剂为B2O3，含量为8wt.%，氮化硼为余量，几种粉体混合均匀。
将混合后的粉末装入石墨模具中，进行热压烧结。
热压烧结步骤中，低温保持步骤为600℃，保温时间为1.5小时；中温保压步骤为1300℃，压力18MPa，保压时间为2小时；高温保压步骤为1800℃，压力20MPa，保压时间为2小时。
将烧结完成后的材料取出，得到氮化硼陶瓷材料。
实施例2
准备氮化硼基粉体，其中添加剂为Si4N3，含量为20wt.%，助烧剂为B2O3，含量为8wt.%，氮化硼为余量，几种粉体混合均匀。
将混合后的粉末装入石墨模具中，进行热压烧结。
热压烧结步骤中，低温保持步骤为800℃，保温时间为1.5小时；中温保压步骤为1200℃，压力20MPa，保压时间为2小时；高温保压步骤为1900℃，压力18MPa，保压时间为1.5小时。
将烧结完成后的材料取出，得到氮化硼陶瓷材料。
实施例3
准备氮化硼基粉体，其中添加剂为CaO，含量为18wt.%，助烧剂为B2O3，含量为8wt.%，氮化硼为余量，几种粉体混合均匀。
将混合后的粉末装入石墨模具中，进行热压烧结。
热压烧结步骤中，低温保持步骤为700℃，保温时间为1.5小时；中温保压步骤为1500℃，压力18MPa，保压时间为2小时；高温保压步骤为1900℃，压力20MPa，保压时间为1.2小时。
将烧结完成后的材料取出，得到氮化硼陶瓷材料。
实施例4
准备氮化硼基粉体，其中添加剂为SiC+Y2O3，含量分别为5wt.%与12wt.%，助烧剂为B2O3，含量为8wt.%，氮化硼为余量，几种粉体混合均匀。
将混合后的粉末装入石墨模具中，进行热压烧结。
热压烧结步骤中，低温保持步骤为700℃，保温时间为1.5小时；中温保压步骤为1400℃，压力18MPa，保压时间为1.5小时；高温保压步骤为1600℃，压力20MPa，保压时间为2小时。
将烧结完成后的材料取出，得到氮化硼陶瓷材料。
以上仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，其特征在于，所述方法包括以下步骤：
（1）将含有添加剂和祝烧剂的BN基粉体混合造粒；
（2）将混合后的粉末装入环形石墨模具中，进行分步热压烧结；
（3）烧结后得到氮化硼陶瓷材料；
所述环形石墨模具包括内环与外环，内环与外环之间缝隙为5~20mm。
2.一种如权利要求1所述的一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，其特征在于，所述分步热压烧结的工艺包括低温保持步骤，中温保压步骤以及高温保压步骤；
所述低温保持步骤为500~800℃，保温时间为0.5~2小时；
所述中温保压步骤为1000~1500℃，压力15~20MPa，保压时间为0.5~2小时；
所述高温保压步骤为1600~1900℃，压力16~25MPa，保压时间为1~3小时；
所述制备方法中，低温在真空下进行，中温在氮气气氛下进行，高温在惰性气氛下进行。
3.一种如权利要求1所述的一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，其特征在于，所述添加剂包括CaO、SiC、Si3N4、ZrO2、Al2O3、Y2O3中的一种或多种，助烧剂为B2O3。
4.一种如权利要求3所述的一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法，其特征在于，所述添加剂含量为15~30wt.%，助烧剂含量为5~10wt.%。
CN201610642334.8A 2016-08-04 2016-08-04 一种利用环形石墨模具分步烧结制备氮化硼陶瓷材料的方法 Pending CN106278284A (zh)

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