CN113135761A - 一种低品位硅藻土制备氮化硅陶瓷的方法 - Google Patents

一种低品位硅藻土制备氮化硅陶瓷的方法 Download PDF

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CN113135761A
CN113135761A CN202110465026.3A CN202110465026A CN113135761A CN 113135761 A CN113135761 A CN 113135761A CN 202110465026 A CN202110465026 A CN 202110465026A CN 113135761 A CN113135761 A CN 113135761A
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silicon nitride
diatomite
low
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姜永久
赵颖
于工
黄旭
王宇
王义鹏
王继涛
王继波
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Linjiang City Baojian Nano Composite Mstar Technology Ltd
Baishan science and technology research institute
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Linjiang City Baojian Nano Composite Mstar Technology Ltd
Baishan science and technology research institute
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Abstract

本发明涉及一种低品位硅藻土制备氮化硅陶瓷的方法，属于氮化硅陶瓷制备技术领域。本发明的低品位硅藻土制备氮化硅陶瓷的方法，先将硅藻土纯化，然后制备氮化硅粉末，再制备氮化硅坯体，最后制备氮化硅陶瓷。本发明的低品位硅藻土制备氮化硅陶瓷的方法用低品位硅藻土代替硅粉做制备氮化硅陶瓷的原材料，不仅成本低，工艺简单，且制备的氮化硅陶瓷性能优异，密度平均值为3.26g/cm3，弯曲强度平均值为537MPa，压缩强度平均值为2139MPa。

Description

一种低品位硅藻土制备氮化硅陶瓷的方法
技术领域
本发明属于氮化硅陶瓷制备技术领域，具体涉及一种低品位硅藻土制备氮化硅陶瓷的方法。
背景技术
氮化硅是一种重要的结构陶瓷材料，具备优异的性能，如(1)机械强度高，硬度接近于刚玉。(2)表面摩擦系数小、耐磨损、弹性模量大，耐高温。(3)热膨胀系数小，导热系数大，抗热震性好。(4)密度低，比重小。(5)耐腐蚀，抗氧化。(6)电绝缘性好。
氮化硅陶瓷的优异性能对于高温、高速、强腐蚀介质的工作环境，具有特殊的使用价值，如氮化硅涡轮转子已应用于装甲车、赛车等特种车辆；氮化硅切削刀具、氮化硅轴承等也在现代化工业制造业中广泛应用。
氮化硅陶瓷制品的生产方法有两种，即反应烧结法和热压烧结法。反应烧结法是将硅粉或硅粉与氮化硅粉的混合料按一般陶瓷制品生产方法成型；然后在氮化炉内，1150～1200℃预氮化，获得一定强度后，可在机床上进行机械加工，接着在1350～1450℃进一步氮化18～36h，直到全部变为氮化硅为止。反应烧结法(RS)适于制造形状复杂，尺寸精确的零件，成本也低，但氮化时间很长。热压烧结法则是将氮化硅粉与少量添加剂(如MgO、Al2O3、MgF2、AlF3或Fe2O3等)，在19.6MPa以上的压力和1600～1700℃条件下压热成型烧结，通常热压烧结法制得的产品比反应烧结制得的产品密度高，性能好。
我国有大量的二三级硅藻土资源，若能利用硅藻土替代硅粉和氮化硅制备氮化硅具有很大的现实意义。
发明内容
有鉴于此，本发明提供一种低品位硅藻土制备氮化硅陶瓷的方法。
本发明实现上述目的采取的技术方案如下。
本发明提供一种低品位硅藻土制备氮化硅陶瓷的方法，步骤如下：
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；
所述低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；
所述纯化后的硅藻土中SiO2含量≥90％；
步骤二、氮化硅坯体的制备
将步骤一所得纯化后硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具中，压制成氮化硅坯体；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气，先以3-5℃/min的升温速度升温至1100℃，保温2-3h，然后以8-10℃/min升温速度升温至1420℃，保温4-5h，再以5-10℃/min降温速度降温至室温，即得到氮化硅陶瓷。
优选的是，所述步骤一中，分散剂为六偏磷酸钠。
优选的是，所述步骤二中，压制压力为15-30MPa，压制时间为120-360s；更进一步的，压制压力为25Mpa，压制时间为240s。
优选的是，所述步骤三中，高纯氮气的纯度为99.9％以上。
优选的是，所述步骤三中，烘干温度为100℃，烘干时间为3h。
与现有技术相比，本发明的有益效果为：
本发明的低品位硅藻土制备氮化硅陶瓷的方法用低品位硅藻土代替硅粉做原材料，不仅成本低，工艺简单，且制备氮化硅陶瓷性能优异，密度平均值为3.26g/cm3，弯曲强度平均值为537MPa，压缩强度平均值为2139MPa。
具体实施方式
为了进一步了解本发明，下面结合具体实施方式对本发明的优选实施方案进行描述，但是应当理解，这些描述只是为进一步说明本发明的特征和优点而不是对本发明专利要求的限制。
本发明的低品位硅藻土制备氮化硅陶瓷的方法，步骤如下：
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性(pH＝7)，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；纯化后的硅藻土中SiO2含量≥90％；分散剂为六偏磷酸钠；
步骤二、氮化硅坯体的制备
将步骤一所得纯化后硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具中，压制成氮化硅坯体，压制压力为15-30MPa，压制时间为120-360s；优选压制压力为25Mpa，压制时间为240s；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气(99.9％)，先以3-5℃/min的升温速度升温至1100℃，保温2-3h，然后以8-10℃/min升温速度升温至1420℃，保温4-5h，再以5-10℃/min降温速度降温至室温，即得到氮化硅陶瓷。
在本发明中所使用的术语，一般具有本领域普通技术人员通常理解的含义，除非另有说明。为了使本领域的技术人员更好地理解本发明的技术方案，下面将结合实施例对本发明作进一步的详细介绍。
在以下实施例中，未详细描述的各种过程和方法是本领域中公知的常规方法。下述实施例中所用的材料、试剂、装置、仪器、设备等，如无特殊说明，均可从商业途径获得。
以下结合实施例进一步说明本发明。
实施例1
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；纯化后的硅藻土中SiO2含量≥90％；分散剂为六偏磷酸钠；
步骤二、氮化硅坯体的制备
将纯化后的硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具(圆片
Figure BDA0003043466430000031
)中，压制压力为20MPa，压制时间为120s；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气(99.9％)，先以4℃/min的升温速度升温至1100℃，保温2.5h，然后以10℃/min升温速度升温至1420℃，保温4h，再以8℃/min的降温速度降温至室温，即得到氮化硅陶瓷。
实施例2
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；纯化后的硅藻土中SiO2含量≥90％；分散剂为六偏磷酸钠；
步骤二、氮化硅坯体的制备
将纯化后的硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具(片15×15×18mm)中，压制成氮化硅坯体，压制压力为25Mpa，压制时间为240s；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气(99.9％)，先以3.5℃/min的升温速度升温至1100℃，保温3h，然后以9℃/min升温速度升温至1420℃，保温4.5h，再以6℃/min的降温速度降温至室温，即得到氮化硅陶瓷。
实施例3
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；纯化后的硅藻土中SiO2含量≥90％；分散剂为六偏磷酸钠；
步骤二、氮化硅坯体的制备
将纯化后的硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具(块20×20×20mm)中，压制成氮化硅坯体，压制压力为30Mpa，压制时间为180s；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气(99.9％)，先以3℃/min的升温速度升温至1100℃，保温3h，然后以8℃/min升温速度升温至1420℃，保温5h，再以5℃/min的降温速度降温至室温，即得到氮化硅陶瓷。
实施例4
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；纯化后的硅藻土中SiO2含量≥90％；分散剂为六偏磷酸钠；
步骤二、氮化硅坯体的制备
将纯化后的硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具(块20×20×20mm)中，压制成氮化硅坯体，压制压力为15Mpa，压制时间为360s；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气(99.9％)，先以5℃/min的升温速度升温至1100℃，保温2h，然后以8℃/min升温速度升温至1420℃，保温5h，再以10℃/min的降温速度降温至室温，即得到氮化硅陶瓷。
对实施例2制备的氮化硅陶瓷的性能进行检测。检测标准：弯曲强度依据GB/T6569-2006测试，压缩强度按照GB/T 8489-2006测试，体积密度按照GB/T25995-2010检测。检测样品十个。测试结果如表1所示。
表1实施例2的氮化硅陶瓷的检测结果
Figure BDA0003043466430000051
Figure BDA0003043466430000061
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (6)

1.一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，步骤如下：
步骤一、硅藻土纯化
将低品位硅藻土预加热到500℃，保温2h，加入2wt％的分散剂擦洗后，用50wt％的硫酸酸洗，100℃保温2h后，水洗至中性，抽滤，干燥，粉碎至粒度≤40微米，得到纯化后的硅藻土；
所述低品位硅藻土为SiO2含量大于75％，小于85％的硅藻土；
所述纯化后的硅藻土中SiO2含量≥90％；
步骤二、氮化硅坯体的制备
将步骤一所得纯化后硅藻土与5wt％聚乙烯醇和7wt％氧化钇混合均匀，置于模具中，压制成氮化硅坯体；
步骤三、氮化硅陶瓷的制备
将氮化硅坯体放入电炉中，通入高纯氮气，先以3-5℃/min的升温速度升温至1100℃，保温2-3h，然后以8-10℃/min升温速度升温至1420℃，保温4-5h，再以5-10℃/min降温速度降温至室温，即得到氮化硅陶瓷。
2.根据权利要求1所述的一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，所述步骤一中，分散剂为六偏磷酸钠。
3.根据权利要求1所述的一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，所述步骤二中，压制压力为15-30MPa，压制时间为120-360s。
4.根据权利要求3所述的一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，所述步骤二中，压制压力为25Mpa，压制时间为240s。
5.根据权利要求1所述的一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，所述步骤三中，高纯氮气的纯度为99.9％以上。
6.根据权利要求1所述的一种低品位硅藻土制备氮化硅陶瓷的方法，其特征在于，所述步骤三中，烘干温度为100℃，烘干时间为3h。
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