CN106187208A - 一种含纳米石墨的大功率led散热氮化铝陶瓷基板 - Google Patents
一种含纳米石墨的大功率led散热氮化铝陶瓷基板 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 239000000758 substrate Substances 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 21
- 239000010439 graphite Substances 0.000 title claims abstract description 21
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 19
- 238000001816 cooling Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910017083 AlN Inorganic materials 0.000 claims abstract description 18
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000002608 ionic liquid Substances 0.000 claims abstract description 10
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- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 6
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
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- 150000002148 esters Chemical class 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，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，提高了各原料的分散性和结合性，此外本发明以铝硅溶胶‑聚乙烯醇、氧化石墨烯等原料的混合浆料作为粘接剂，对各原料的浸润性佳，且热稳定性好，降低烧结氛的氧含量，提高氮化铝晶格纯净度，加入的纳米石墨能提高陶瓷体内部的润滑性，提高材料的耐磨损、抗热压能力；这种陶瓷基板具有良好导热效果和优良力学性能，表面致密光滑，不易开裂破损，其用于大功率LED芯片基板时极大地延长了芯片的使用寿命，具有良好的市场效益。
Description
技术领域
本发明涉及氮化铝陶瓷技术领域，尤其涉及一种含纳米石墨的大功率LED散热氮化铝陶瓷基板。
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，提供一种含纳米石墨的大功率LED散热氮化铝陶瓷基板。
本发明是通过以下技术方案实现的：
一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，该陶瓷基板由以下重量份的原料制成：氮化铝40-50、纳米氮化铝8-12、纳米石墨0.4-0.5、氧化钇2-3、氧化石墨烯0.1-0.2、聚乙烯醇1-2、离子液体10-15、碳酸钾0.1-0.2、异丙醇铝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。
所述的一种含纳米石墨的大功率LED散热氮化铝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，随后再加入聚乙烯醇、氧化石墨烯、碳酸钾，继续搅拌混合40-50min后备用。
（4）将纳米氮化铝、纳米石墨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5000-6000mPa.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400-500℃，保温排胶5-6h，随后在1620-1680℃条件下真空保温烧结4-6h，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，提高了各原料的分散性和结合性，此外本发明以铝硅溶胶-聚乙烯醇、氧化石墨烯等原料的混合浆料作为粘接剂，这种粘接剂粘接效果良好，对各原料的浸润性佳，且热稳定性好，其中的有效成分还能降低烧结氛的氧含量，提高氮化铝晶格纯净度，加入的纳米石墨能提高陶瓷体内部的润滑性，提高材料的耐磨损、抗热压能力；本发明制得的氮化铝陶瓷基板具有良好导热效果和优良力学性能，表面致密光滑，不易开裂破损，其用于大功率LED芯片基板时极大地延长了芯片的使用寿命，具有良好的市场效益。
具体实施方式
一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，该陶瓷基板由以下重量份的原料制成：氮化铝40、纳米氮化铝8、纳米石墨0.4、氧化钇2、氧化石墨烯0.1、聚乙烯醇1、离子液体10、碳酸钾0.1、异丙醇铝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，随后再加入聚乙烯醇、氧化石墨烯、碳酸钾，继续搅拌混合40min后备用。
（4）将纳米氮化铝、纳米石墨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5500mPa.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400℃，保温排胶5h，随后在1620℃条件下真空保温烧结4h，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：3.30g.cm-3；导热率：190.2W/(mk)；表面粗糙度Rmax≤0.2μm；抗弯强度：410MPa；断裂韧性：3.12±0.05MPa.m1/2。
Claims (5)
1.一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，其特征在于，该陶瓷基板由以下重量份的原料制成：氮化铝40-50、纳米氮化铝8-12、纳米石墨0.4-0.5、氧化钇2-3、氧化石墨烯0.1-0.2、聚乙烯醇1-2、离子液体10-15、碳酸钾0.1-0.2、异丙醇铝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所述的一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，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所述的一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，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所述的一种含纳米石墨的大功率LED散热氮化铝陶瓷基板，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所述的一种含纳米石墨的大功率LED散热氮化铝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，随后再加入聚乙烯醇、氧化石墨烯、碳酸钾，继续搅拌混合40-50min后备用；
（4）将纳米氮化铝、纳米石墨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5000-6000mPa.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400-500℃，保温排胶5-6h，随后在1620-1680℃条件下真空保温烧结4-6h，出料后即得。
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| CN110650802A (zh) * | 2017-05-18 | 2020-01-03 | 高保真生物技术有限公司 | 用于制造微通道阵列的方法 |
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| CN102030538A (zh) * | 2009-09-30 | 2011-04-27 | 比亚迪股份有限公司 | 氮化铝陶瓷的制备方法及采用该方法制备的氮化铝陶瓷 |
| CN105367110A (zh) * | 2015-10-27 | 2016-03-02 | 合肥龙多电子科技有限公司 | 一种硫酸钙晶须弥散增强的高导热氮化铝-碳化硅复合电路板基板材料及其制备方法 |
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| CN105367110A (zh) * | 2015-10-27 | 2016-03-02 | 合肥龙多电子科技有限公司 | 一种硫酸钙晶须弥散增强的高导热氮化铝-碳化硅复合电路板基板材料及其制备方法 |
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| CN106587970A (zh) * | 2016-12-16 | 2017-04-26 | 东莞市翔龙能源科技有限公司 | 一种辐射散热的led陶瓷基板及其制备方法 |
| CN110650802A (zh) * | 2017-05-18 | 2020-01-03 | 高保真生物技术有限公司 | 用于制造微通道阵列的方法 |
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