CN106242578A - 一种石墨烯增韧的大功率led散热陶瓷基板 - Google Patents

一种石墨烯增韧的大功率led散热陶瓷基板 Download PDF

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CN106242578A
CN106242578A CN201610574235.0A CN201610574235A CN106242578A CN 106242578 A CN106242578 A CN 106242578A CN 201610574235 A CN201610574235 A CN 201610574235A CN 106242578 A CN106242578 A CN 106242578A
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陆厚平
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Abstract

本发明公开了一种石墨烯增韧的大功率LED散热陶瓷基板，该陶瓷基板使用离子液体和去离子水混合作为溶剂介质，取代了传统的流延成型工艺中的有毒有机溶剂，提高氮化铝与其他原料间的浸润性，纳米材料的分散性得到提高，改性效果显著；此外，本发明利用铝硅溶胶结合陶瓷料，流延效果好，还可有效的降低烧结氛围内的氧含量，防止其向氮化铝晶格内部扩散，从而提高其导热性，此外加入的石墨烯有增强、增韧等功效，降低氮化铝陶瓷的脆性，最终制得的氮化铝陶瓷基板具有良好的导热性，且坚韧致密，不易损坏，使用性能更佳。

Description

一种石墨烯增韧的大功率LED散热陶瓷基板
技术领域
本发明涉及氮化铝陶瓷技术领域，尤其涉及一种石墨烯增韧的大功率LED散热陶瓷基板。
背景技术
大功率LED芯片产生的热量不能及时有效的散失，将严重影响LED的发射光谱、发光强度、封装材料性能、芯片的寿命等，因此，大功率LED的散热问题一直是固态照明行业的一大技术瓶颈，在传统封装工艺生产的LED中，基板散热因其直接有效的散热优势成为国内外重点研究的对象。目前研究应用较多的为铝基散热基板，然而，随着LED散热需求的提升，铝基板的缺陷也逐步表现出来，其内部的绝缘层导致整体散热性差，容易结温，从而降低灯具的使用寿命。相比于铝基板散热套件，陶瓷散热基板具有高绝缘性、高热辐射、高导热、电磁兼容性好等优点成为备受瞩目的一种替代材料，其中氮化铝陶瓷是综合性能较为理想的封装材料，然而，在实际应用中氮化铝陶瓷存在烧结温度高，导热性能较差等缺陷，制约着产品的推广应用。
《Y2O3和纳米AlN协同作用对氮化铝陶瓷烧结性能及热传导的影响》一文介绍了以Y2O3作为烧结助剂与纳米氮化铝协同作用在低烧结温度下制成了较高导热系数的氮化铝陶瓷，这种方法虽然一定程度的提高了氮化铝陶瓷的致密度，但是其导热系数仍有待提高，且纳米粉体的添加量必须受到严格的控制，需要在较高的烧结温度下才能改善氮化铝陶瓷的性能。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种石墨烯增韧的大功率LED散热陶瓷基板。
本发明是通过以下技术方案实现的：
一种石墨烯增韧的大功率LED散热陶瓷基板，该陶瓷基板由以下重量份的原料制成：氮化铝30-40、纳米氮化铝15-20、氧化钇1-2、石墨烯0.3-0.5、离子液体10-15、异丙醇铝0.1-0.2、六偏磷酸钠0.1-0.2、正硅酸乙酯0.4-0.5、去离子水20-25，适量的稀硝酸溶液。
所述的氮化铝的氧含量为0.5-1.5wt.%，D50粒径为0.5-2μm。
所述的氧化钇纯度大于99.99%，D50粒径为0.1-0.5μm。
所述的离子液体为水溶性离子液体。
所述的一种石墨烯增韧的大功率LED散热陶瓷基板的制备方法分为以下几个步骤：
（1）先将异丙醇铝与8-10重量份的去离子水混合，置于90℃水浴条件下，磁力搅拌混合，待混合液的pH值不再变化为止，随后加入稀硝酸溶液，调节体系pH值为4.0-5.0，随后水浴升温至100℃，继续回流1-1.5h得到稳定的铝溶胶备用。
（2）将正硅酸乙酯与余量的去离子水混合，在50-60℃的水浴中超声反应20-30min，随后滴加稀硝酸溶液，调节溶液pH值为4.0-5.0，反应40-50min后得硅溶胶备用。
（3）将步骤（1）制备的铝溶胶加热至80-85℃，缓慢加入步骤（2）制备的硅溶胶，边加边搅拌，随后再加入六偏磷酸钠，继续搅拌混合40-50min后备用。
（4）将纳米氮化铝、石墨烯与离子液体混合球磨20-30min，随后将其与氮化铝、氧化钇混合，继续球磨分散3-5h，最后再将其与步骤（3）制得的物料混合，再次球磨分散10-15h，球磨结束后所得浆料真空脱泡，控制粘度为5000-8000mPa.s，所得浆料进行流延处理，控制厚度，得到胚体。
（5）将制得的胚体在承烧板上以1-2℃/min的升温速率升温至500-600℃，保温排胶5-6h，随后在1600-1700℃条件下真空保温烧结5-6h，出料后即得。
本发明优点在于，使用离子液体和去离子水混合作为溶剂介质，取代了传统的流延成型工艺中的有毒有机溶剂，提高氮化铝与其他原料间的浸润性，纳米材料的分散性得到提高，改性效果显著；此外，本发明利用铝硅溶胶结合陶瓷料，流延效果好，还可有效的降低烧结氛围内的氧含量，防止其向氮化铝晶格内部扩散，从而提高其导热性，此外加入的石墨烯有增强、增韧等功效，降低氮化铝陶瓷的脆性，最终制得的氮化铝陶瓷基板具有良好的导热性，且坚韧致密，不易损坏，使用性能更佳。
具体实施方式
一种石墨烯增韧的大功率LED散热陶瓷基板，该陶瓷基板由以下重量份的原料制成：氮化铝30、纳米氮化铝15、氧化钇1、石墨烯0.3、离子液体10、异丙醇铝0.1、六偏磷酸钠0.1、正硅酸乙酯0.4、去离子水20，适量的稀硝酸溶液。
其中氮化铝的氧含量为0.5wt.%，D50粒径为0.5μm。
其中氧化钇纯度大于99.99%，D50粒径为0.1μm。
其中离子液体为水溶性离子液体。
该实施例陶瓷基板由以下几个步骤制备得到：
（1）先将异丙醇铝与8重量份的去离子水混合，置于90℃水浴条件下，磁力搅拌混合，待混合液的pH值不再变化为止，随后加入稀硝酸溶液，调节体系pH值为4.0，随后水浴升温至100℃，继续回流1h得到稳定的铝溶胶备用。
（2）将正硅酸乙酯与余量的去离子水混合，在50℃的水浴中超声反应20min，随后滴加稀硝酸溶液，调节溶液pH值为4.0，反应40min后得硅溶胶备用。
（3）将步骤（1）制备的铝溶胶加热至80℃，缓慢加入步骤（2）制备的硅溶胶，边加边搅拌，随后再加入六偏磷酸钠，继续搅拌混合40min后备用。
（4）将纳米氮化铝、石墨烯与离子液体混合球磨20min，随后将其与氮化铝、氧化钇混合，继续球磨分散3h，最后再将其与步骤（3）制得的物料混合，再次球磨分散10h，球磨结束后所得浆料真空脱泡，控制粘度为6500mPa.s，所得浆料进行流延处理，得到厚度为0.55mm的胚体。
（5）将制得的胚体在承烧板上以1℃/min的升温速率升温至500℃，保温排胶5h，随后在1650℃条件下真空保温烧结5h，出料后即得。
该陶瓷基板根据相应标准测试得到的各项性能指标如下：
密度：3.24g.cm-3；导热率：184.5W/(mk)；表面粗糙度Rmax≤0.2μm；抗弯强度：378.2MPa；断裂韧性：3.02±0.05MPa.m1/2。

Claims (5)

1.一种石墨烯增韧的大功率LED散热陶瓷基板，其特征在于，该陶瓷基板由以下重量份的原料制成：氮化铝30-40、纳米氮化铝15-20、氧化钇1-2、石墨烯0.3-0.5、离子液体10-15、异丙醇铝0.1-0.2、六偏磷酸钠0.1-0.2、正硅酸乙酯0.4-0.5、去离子水20-25，适量的稀硝酸溶液。
2.如权利要求1所述的一种石墨烯增韧的大功率LED散热陶瓷基板，其特征在于，所述的氮化铝的氧含量为0.5-1.5wt.%，D50粒径为0.5-2μm。
3.如权利要求1所述的一种石墨烯增韧的大功率LED散热陶瓷基板，其特征在于，所述的氧化钇纯度大于99.99%，D50粒径为0.1-0.5μm。
4.如权利要求1所述的一种石墨烯增韧的大功率LED散热陶瓷基板，其特征在于，所述的离子液体为水溶性离子液体。
5.如权利要求1所述的一种石墨烯增韧的大功率LED散热陶瓷基板的制备方法分为以下几个步骤：
（1）先将异丙醇铝与8-10重量份的去离子水混合，置于90℃水浴条件下，磁力搅拌混合，待混合液的pH值不再变化为止，随后加入稀硝酸溶液，调节体系pH值为4.0-5.0，随后水浴升温至100℃，继续回流1-1.5h得到稳定的铝溶胶备用；
（2）将正硅酸乙酯与余量的去离子水混合，在50-60℃的水浴中超声反应20-30min，随后滴加稀硝酸溶液，调节溶液pH值为4.0-5.0，反应40-50min后得硅溶胶备用；
（3）将步骤（1）制备的铝溶胶加热至80-85℃，缓慢加入步骤（2）制备的硅溶胶，边加边搅拌，随后再加入六偏磷酸钠，继续搅拌混合40-50min后备用；
（4）将纳米氮化铝、石墨烯与离子液体混合球磨20-30min，随后将其与氮化铝、氧化钇混合，继续球磨分散3-5h，最后再将其与步骤（3）制得的物料混合，再次球磨分散10-15h，球磨结束后所得浆料真空脱泡，控制粘度为5000-8000mPa.s，所得浆料进行流延处理，控制厚度，得到胚体；
（5）将制得的胚体在承烧板上以1-2℃/min的升温速率升温至500-600℃，保温排胶5-6h，随后在1600-1700℃条件下真空保温烧结5-6h，出料后即得。
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