CN116606146A - 一种高良品率的氮化硅基板及其制备方法 - Google Patents

一种高良品率的氮化硅基板及其制备方法 Download PDF

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CN116606146A
CN116606146A CN202310600108.3A CN202310600108A CN116606146A CN 116606146 A CN116606146 A CN 116606146A CN 202310600108 A CN202310600108 A CN 202310600108A CN 116606146 A CN116606146 A CN 116606146A
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silicon nitride
oxide
nitride substrate
parts
high yield
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杨文伍
喻大钊
王进科
任莉
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Ningbo Silver Porcelain New Material Co ltd
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Abstract

本发明提供一种高良品率的氮化硅基板及其制备方法，涉及陶瓷材料制备技术领域。该一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅70‑95份、烧助结剂8‑16份、表面活性剂8‑12份、碳化钨2‑15份、粘结剂2‑6份，优选的，所述烧结助剂为液相烧结，液相烧结体系以氧化铝‑三氧化二钇，氮化铝‑Re2O3，为主的液相烧结体系，其中Re2O3通常是三氧化二钇、氧化镱、氧化钪和氧化镥等稀土元素的氧化物。通过碳化钨与氧化物的组合，有效地提高烧结过程的致密过程，并且碳化钨在烧结过程中不转变为液相，可有效抑制氮化硅因为液相太多而导致的烧结过程变形问题，从而避免翘曲等不良品的产生。

Description

一种高良品率的氮化硅基板及其制备方法
技术领域
本发明涉及陶瓷材料制备技术领域，具体为一种高良品率的氮化硅基板及其制备方法。
背景技术
功率电子器件在电力存储，电力输送，电动汽车，电力机车等众多工业领域得到越来越广泛的应用，随着功率电子器件本身不断地大功率化和高集成化，芯片在工作过程中将会产生大量的热，如果这些热量不能及时有效地发散出去，功率电子器件的工作性能将会受到影响，严重的话，功率电子器件本身会被破损，这就要求担负绝缘和散热功能的陶瓷基板封装材料必须具备卓越的机械性能和导热性能，氮化硅(Si 3N4)具有强度高、韧性好、耐热冲击、耐腐蚀和耐磨损等性能，在航空航天、机械、核能、化工、海洋工程、装甲防护等领域具有广泛的应用。
基板材料被广泛运用于汽车、航空及半导体行业，氮化硅基板材料因具有综合力学性能好、耐腐蚀等特点而被广泛应用。
目前，氮化硅基板在加工过程中，所加工的步骤、工艺和材料都比较复杂，加工得到的氮化硅基板的合格率不高，为了解决上述问题需要一种高良品率的氮化硅基板及其制备方法。
发明内容
针对现有技术的不足，本发明提供了一种高良品率的氮化硅基板及其制备方法，解决了氮化硅基板在加工过程中，所加工的步骤、工艺和材料都比较复杂，加工得到的氮化硅基板的合格率不高的问题。
为实现以上目的，本发明通过以下技术方案予以实现：一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅70-95份、烧助结剂8-16份、表面活性剂8-12份、碳化钨2-15份、粘结剂2-6份。
优选的，所述烧结助剂为液相烧结，液相烧结体系以氧化铝-三氧化二钇，氮化铝-Re2O3，为主的液相烧结体系，其中Re2O3通常是三氧化二钇、氧化镱、氧化钪和氧化镥等稀土元素的氧化物。
优选的，所述添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
优选的，一种高良品率的氮化硅基板的制备方法，包括以下步骤：
步骤一：取出所需的氮化硅研磨，冷却后得到粉末；
步骤二：将粉末与添加剂和20％的去离子水进行混合；
步骤三：将混合料进行搅拌，搅拌过程中依次加入表面活性剂、烧结助剂、粘结剂、硅烷偶联剂、加强剂和余下去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，然后在惰性气体环境下进行预烧结，升温到预定温度后进行高温烧结作业，并保温指定时间后降温到常温状态，从而得到氮化硅基板材料；
步骤六：将氮化硅基板材料进行清洗，通过烘干设备进行烘干，再由检验人员进行检验核查，从而得到合格的产品，不合格的产品进行粉碎后进行研磨，将研磨得到的粉状物体通过步骤一继续进行加工。
优选的，步骤一中，所述研磨用的设备转速为600-1400r/mi n，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
优选的，步骤二中，所述搅拌的转速控制在80-130r/mi n。
优选的，步骤三中，所述搅拌的转速控制在150-200r/mi n。
优选的，步骤四中，所述挤压的压力为50-300MPa，压制时间为4-8mi n。
优选的，步骤五中，所述排胶设备的作业环境为真空环境，温度范围控制在300-500℃，保温时间4-6h。
本发明提供了一种高良品率的氮化硅基板及其制备方法。具备以下有益效果：
本发明通过碳化钨与氧化物的组合，有效地提高烧结过程的致密过程，并且碳化钨在烧结过程中不转变为液相，可有效抑制氮化硅因为液相太多而导致的烧结过程变形问题，从而避免翘曲等不良品的产生。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一：
本发明实施例提供一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅70-95份、烧助结剂8-16份、表面活性剂8-12份、碳化钨2-15份、粘结剂2-6份。
所述烧结助剂为液相烧结，液相烧结体系以氧化铝-三氧化二钇，氮化铝-Re2O3，为主的液相烧结体系，其中Re2O3通常是三氧化二钇、氧化镱、氧化钪和氧化镥等稀土元素的氧化物。
所述添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
一种高良品率的氮化硅基板的制备方法，包括以下步骤：
步骤一：取出所需的氮化硅研磨，冷却后得到粉末；
步骤二：将粉末与添加剂和20％的去离子水进行混合；
步骤三：将混合料进行搅拌，搅拌过程中依次加入表面活性剂、烧结助剂、粘结剂、硅烷偶联剂、加强剂和余下去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，然后在惰性气体环境下进行预烧结，升温到预定温度后进行高温烧结作业，并保温指定时间后降温到常温状态，从而得到氮化硅基板材料；
步骤六：将氮化硅基板材料进行清洗，通过烘干设备进行烘干，再由检验人员进行检验核查，从而得到合格的产品，不合格的产品进行粉碎后进行研磨，将研磨得到的粉状物体通过步骤一继续进行加工。
步骤一中，所述研磨用的设备转速为600-1400r/mi n，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
步骤二中，所述搅拌的转速控制在80-130r/mi n。
步骤三中，所述搅拌的转速控制在150-200r/mi n。
步骤四中，所述挤压的压力为50-300MPa，压制时间为4-8mi n。
步骤五中，所述排胶设备的作业环境为真空环境，温度范围控制在300-500℃，保温时间4-6h。
实施例二：
本发明实施例提供一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅60-80份、添加剂8-16份、去离子水3-8份、表面活性剂8-12份、碳纤维15-25份、加强剂2-5份、粘结剂2-6份、硅烷偶联剂2-10份。
添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
一种高良品率的氮化硅基板的制备方法，应用于权利要求1-3的一种高良品率的氮化硅基板，包括以下步骤：
步骤一：取出所需的氮化硅研磨并进行脱氧处理，冷却后得到粉末；
步骤二：将粉末与碳纤维、钨纤维和20％的去离子水进行混合，混合过程中依次加入钴、铁、锰和镍；
步骤三：将混合料进行搅拌，搅拌过程中依次加入添加剂、表面活性剂、粘结剂、硅烷偶联剂、加强剂和余下80％的去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，从而得到氮化硅基板材料；
步骤六：将氮化硅基板材料进行清洗，通过烘干设备进行烘干，再由检验人员进行检验核查，从而得到合格的产品，不合格的产品进行粉碎后进行研磨，将研磨得到的粉状物体通过步骤一继续进行加工。
步骤一中，研磨用的设备转速为600-1400r/mi n，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
步骤二中，搅拌的转速控制在80-130r/mi n。
步骤三中，搅拌的转速控制在150-200r/mi n。
步骤四中，挤压的压力为300-500MPa，压制时间为4-8mi n。
步骤五中，排胶设备的作业环境为真空环境，温度范围控制在300-500℃，保温时间4-6h。
实施例三：
本发明实施例提供一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅60-80份、添加剂8-16份、去离子水3-8份、表面活性剂8-12份、碳纤维15-25份、加强剂2-5份、粘结剂2-6份、硅烷偶联剂2-10份。
添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
一种高良品率的氮化硅基板的制备方法，应用于权利要求1-3的一种高良品率的氮化硅基板，包括以下步骤：
步骤一：取出所需的氮化硅研磨并进行脱氧处理，冷却后得到粉末；
步骤二：将粉末与碳纤维、钨纤维和20％的去离子水进行混合；
步骤三：将混合料进行搅拌，搅拌过程中依次加入添加剂、表面活性剂、粘结剂、硅烷偶联剂、加强剂和余下80％的去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，从而得到氮化硅基板材料；
步骤六：将氮化硅基板材料进行清洗，通过烘干设备进行烘干，再由检验人员进行检验核查，从而得到合格的产品，不合格的产品进行粉碎后进行研磨，将研磨得到的粉状物体通过步骤一继续进行加工。
步骤一中，研磨用的设备转速为600-1400r/mi n，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
步骤二中，搅拌的转速控制在80-130r/mi n。
步骤三中，搅拌的转速控制在150-200r/mi n。
步骤四中，挤压的压力为300-500MPa，压制时间为4-8mi n。
步骤五中，排胶设备的作业环境为真空环境，温度范围控制在300-500℃，保温时间4-6h。
实施例四：
本发明实施例提供一种高良品率的氮化硅基板，包括以下重量份的原料：氮化硅60-80份、添加剂8-16份、去离子水3-8份、表面活性剂8-12份、碳纤维15-25份、烧结碳化钨颗粒10-15份、加强剂2-5份、粘结剂2-6份、硅烷偶联剂2-10份、烧结助剂12-15份。
烧结助剂分为固相烧结和液相烧结，固相烧结助剂体系以A l-B-C-B4C为主，液相烧结体系以氧化铝-三氧化二钇，氮化铝-三氧化二铼为主的液相烧结体系，其中三氧化二铼通常是三氧化二钇、氧化铒、氧化镱、氧化钪和氧化镥等稀土元素的氧化物。
添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
一种高良品率的氮化硅基板的制备方法，应用于权利要求1-3的一种高良品率的氮化硅基板，包括以下步骤：
步骤一：取出所需的氮化硅研磨并进行脱氧处理，冷却后得到粉末；
步骤二：将粉末与碳纤维、烧结碳化钨颗粒、钨纤维和20％的去离子水进行混合，混合过程中依次加入钴、铁、锰和镍；
步骤三：将混合料进行搅拌，搅拌过程中依次加入添加剂、表面活性剂、烧结助剂、粘结剂、硅烷偶联剂、加强剂和余下80％的去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，然后在惰性气体环境下进行预烧结，升温到预定温度后进行高温烧结作业，并保温指定时间后降温到常温状态，从而得到氮化硅基板材料。
步骤一中，研磨用的设备转速为600-1400r/mi n，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
步骤二中，搅拌的转速控制在80-130r/mi n。
步骤三中，搅拌的转速控制在150-200r/mi n。
步骤四中，挤压的压力为300-500MPa，压制时间为4-8mi n。
通过上述实施例一至实施例四得到的氮化硅基板的合格率计算得到结果如下：
总结：通过碳化钨与氧化物的组合，有效地提高烧结过程的致密过程，并且碳化钨在烧结过程中不转变为液相，可有效抑制氮化硅因为液相太多而导致的烧结过程变形问题，从而避免翘曲等不良品的产生。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (9)

1.一种高良品率的氮化硅基板，其特征在于：包括以下重量份的原料：氮化硅70-95份、烧助结剂8-16份、表面活性剂8-12份、碳化钨2-15份、粘结剂2-6份。
2.根据权利要求1所述的一种高良品率的氮化硅基板，其特征在于：所述烧结助剂为液相烧结，液相烧结体系以氧化铝-三氧化二钇，氮化铝-Re2O3，为主的液相烧结体系，其中Re2O3通常是三氧化二钇、氧化镱、氧化钪和氧化镥等稀土元素的氧化物。
3.根据权利要求1所述的一种高良品率的氮化硅基板，其特征在于：所述添加剂为氧化镁、氧化铝、氟化镁和氧化铁中的一种或多种。
4.一种高良品率的氮化硅基板的制备方法，其特征在于，应用于权利要求1-3所述的一种高良品率的氮化硅基板，包括以下步骤：
步骤一：取出所需的氮化硅研磨，冷却后得到粉末；
步骤二：将粉末与添加剂和20％的去离子水进行混合；
步骤三：将混合料进行搅拌，搅拌过程中依次加入表面活性剂、烧结助剂、粘结剂、硅烷偶联剂、加强剂和余下去离子水再次搅拌混合；
步骤四：将步骤三中的混合物进行造粒，再通过模具和挤压设备进行压制成型，从而得到氮化硅基板的坯体；
步骤五：将坯体进行热机去除，然后在惰性气体环境下进行预烧结，升温到预定温度后进行高温烧结作业，并保温指定时间后降温到常温状态，从而得到氮化硅基板材料；
步骤六：将氮化硅基板材料进行清洗，通过烘干设备进行烘干，再由检验人员进行检验核查，从而得到合格的产品，不合格的产品进行粉碎后进行研磨，将研磨得到的粉状物体通过步骤一继续进行加工。
5.根据权利要求4所述的一种高良品率的氮化硅基板的制备方法，其特征在于：步骤一中，所述研磨用的设备转速为600-1400r/min，脱氧设备的脱氧温度为800-1500℃，脱氧时间为3-5h，脱氧环境为惰性气体环境，惰性气体为氮气或者氩气。
6.根据权利要求1所述的一种高良品率的氮化硅基板的制备方法，其特征在于：步骤二中，所述搅拌的转速控制在80-130r/min。
7.根据权利要求1所述的一种高良品率的氮化硅基板的制备方法，其特征在于：步骤三中，所述搅拌的转速控制在150-200r/min。
8.根据权利要求1所述的一种高良品率的氮化硅基板的制备方法，其特征在于：步骤四中，所述挤压的压力为50-300MPa，压制时间为4-8min。
9.根据权利要求1所述的一种高良品率的氮化硅基板的制备方法，其特征在于：步骤五中，所述排胶设备的作业环境为真空环境，温度范围控制在300-500℃，保温时间4-6h。
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Publication number Priority date Publication date Assignee Title
CN116945353A (zh) * 2023-09-19 2023-10-27 江苏力星通用钢球股份有限公司 一种氮化硅陶瓷球坯的脱胶工艺
CN116945353B (zh) * 2023-09-19 2023-12-08 江苏力星通用钢球股份有限公司 一种氮化硅陶瓷球坯的脱胶工艺

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