CN116239367A - 一种高导热氧化铝陶瓷材料及陶瓷电路基板 - Google Patents
一种高导热氧化铝陶瓷材料及陶瓷电路基板 Download PDFInfo
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052574 oxide ceramic Inorganic materials 0.000 title claims abstract description 18
- 239000000758 substrate Substances 0.000 title claims abstract description 13
- 239000000919 ceramic Substances 0.000 title claims abstract description 11
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims abstract description 37
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 24
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021538 borax Inorganic materials 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 16
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 31
- 239000004917 carbon fiber Substances 0.000 claims description 31
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 31
- 239000004530 micro-emulsion Substances 0.000 claims description 29
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 15
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 14
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 14
- 229920000053 polysorbate 80 Polymers 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- PPYIVKOTTQCYIV-UHFFFAOYSA-L beryllium;selenate Chemical compound [Be+2].[O-][Se]([O-])(=O)=O PPYIVKOTTQCYIV-UHFFFAOYSA-L 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
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- 238000010304 firing Methods 0.000 claims description 2
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- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及陶瓷材料领域，具体为一种高导热氧化铝陶瓷材料及陶瓷电路基板，以重量份数计，制备原料包括以下组成：氧化铝80‑100份、氧化锆12‑16份、氧化铍包覆一维碳材料5‑10份、硼砂5‑10份、尿素1‑5份，本发明所制备的氧化铝陶瓷材料具有良好的导热性能和力学强度，其中，抗弯强度≥573MPa，断裂韧性≥9.8MPa·m1/2，热导率≥54.6W/(m·K)。
Description
技术领域
本发明涉及陶瓷材料领域，具体为一种高导热氧化铝陶瓷材料及陶瓷电路基板。
背景技术
在电子行业，基板的作用是搭载、固定电子元器件，利用表面或内部形成的电路图形，进行电路连接，同时兼有绝缘、导热及保护器件的作用。电子信息工业以及科学技术的发展，对大功率集成电路基板的散热性能以及绝缘性能要求越来越高。陶瓷基板无疑是大功率集成电路最佳的选择之一。
氧化铝是目前广泛应用的中小功率陶瓷基板材料，其机械强度相对较高，来源丰富、价格低廉，但热导率较低，约为20W/(m·K)，远远不能满足LTCC技术背景下，大功率集成电路对电路基板散热性能的需求。
发明内容
发明目的：针对上述技术问题，本发明提出了一种高导热氧化铝陶瓷材料及陶瓷电路基板。
所采用的技术方案如下：
一种高导热氧化铝陶瓷材料，含有氧化铍包覆一维碳材料。
进一步地，以重量份数计，制备原料包括以下组成：
氧化铝80-100份、氧化锆12-16份、氧化铍包覆一维碳材料5-10份、硼砂5-10份、尿素1-5份。
进一步地，所述氧化铍包覆一维碳材料为氧化铍包覆碳纤维或氧化铍包覆碳纳米管。
进一步地，所述氧化铍包覆一维碳材料的制备方法如下：
将水溶性铍盐溶于水中，再加入一维碳材料、环己烷、吐温-80和正丁醇，高速搅拌后得到微乳液A，将浓氨水、环己烷、吐温-80和正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌4-6h后陈化、离心，固体洗涤后再经干燥、煅烧即可。
进一步地，所述一维碳材料预先经过表面粗糙化处理。
进一步地，所述一维碳材料预先经过浓硫酸浸泡。
进一步地，煅烧温度为950-1000℃，煅烧时间为3-5h。
本发明还提供了一种高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨后与氧化铍包覆一维碳材料、硼砂、尿素混合加热至900-1000℃进行预烧，得到的混合物料再次球磨后干燥、造粒，压制成型得到粗坯，所得粗坯升温至1350-1500℃进行高温烧结，所述高温烧结时间为1-4h。
进一步地，预烧在氮气氛围下进行。
本发明还提供了一种陶瓷电路基板，包括上述高导热氧化铝陶瓷材料。
本发明的有益效果：
本发明提供了一种高导热氧化铝陶瓷材料，氧化锆均匀弥散分布在氧化铝基体中，随着温度的变化，氧化锆发生相变，相应的产生体积膨胀和切应变，导致张应力和微裂纹的形成，这些裂纹局限在小尺寸晶粒中，其萌生和扩展等都会消耗外应力场的能量，进而提高陶瓷材料陶瓷的韧性和强度，一维碳材料起到的是短纤维增韧的作用，由于一维碳材料超强的力学性能，在拔出和断裂时，都要消耗更多的能量，有利于阻止陶瓷裂纹的扩展，但是由于一维碳材料在陶瓷基体中易团聚、难分散，难以形成三维导热网络，发明人利用高导热性能的氧化铍对其进行包覆，既有利于一维碳材料在氧化铝基体中的分散，也进一步提高了一维碳材料的导热性能，在热量传递过程中，大部分热量沿着高导热的氧化铍包覆一维碳材料所搭接的高导热网络通道进行高速传递，大大提高氧化铝陶瓷材料的热导率，硼砂和尿素在预烧时能够原位生成氮化硼，其热膨胀系数低，可以填充氧化铝、氧化锆、氧化铍包覆一维碳材料之间的孔隙，提高整体的力学强度，本发明所制备的氧化铝陶瓷材料具有良好的导热性能和力学强度，其中，抗弯强度≥573MPa，断裂韧性≥9.8MPa·m1/2，热导率≥54.6W/(m·K)。
附图说明
图1为本发明实施例1所制备氧化铝陶瓷材料断面的SEM图。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。本发明未提及的技术均参照现有技术。
实施例1：
一种高导热氧化铝陶瓷材料，以重量份数计，制备原料包括以下组成：
氧化铝95份、氧化锆15份、氧化铍包覆碳纤维8份、硼砂6份、尿素3份。
其中，氧化铍包覆碳纤维的制备方法如下：
将碳纤维预先放入浓硫酸中50℃浸泡30min，滤出水洗至中性后烘干待用，将17.7g BeSO4·4H2O溶于100mL水中，再加入20g经过硫酸处理的碳纤维、450mL环己烷、111.6g吐温-80和65mL正丁醇，高速搅拌后得到微乳液A，将100mL浓氨水、450mL环己烷、111.6g吐温-80和65mL正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌5h后陈化、离心，所得固体依次用水、乙醇、丙酮洗涤后，80℃干燥24h、再转移至马弗炉中以10℃/min的速度升温980℃煅烧4h即可。
上述高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨10h后与氧化铍包覆碳纤维、硼砂、尿素混合均匀，氮气氛围下加热至950℃预烧1h，预烧得到的混合物料再次球磨1h后干燥、造粒，50MPa压制成型得到粗坯，所得粗坯升温至1480℃进行高温烧结，高温烧结时间为2h。
实施例2：
一种高导热氧化铝陶瓷材料，以重量份数计，制备原料包括以下组成：
氧化铝100份、氧化锆16份、氧化铍包覆碳纤维10份、硼砂10份、尿素5份。
其中，氧化铍包覆碳纤维的制备方法如下：
将碳纤维预先放入浓硫酸中50℃浸泡30min，滤出水洗至中性后烘干待用，将17.7g BeSO4·4H2O溶于100mL水中，再加入20g经过硫酸处理的碳纤维、450mL环己烷、111.6g吐温-80和65mL正丁醇，高速搅拌后得到微乳液A，将100mL浓氨水、450mL环己烷、111.6g吐温-80和65mL正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌6h后陈化、离心，所得固体依次用水、乙醇、丙酮洗涤后，80℃干燥24h、再转移至马弗炉中以10℃/min的速度升温1000℃煅烧5h即可。
上述高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨10h后与氧化铍包覆碳纤维、硼砂、尿素混合均匀，氮气氛围下加热至1000℃预烧1h，预烧得到的混合物料再次球磨1h后干燥、造粒，50MPa压制成型得到粗坯，所得粗坯升温至1500℃进行高温烧结，高温烧结时间为4h。
实施例3：
一种高导热氧化铝陶瓷材料，以重量份数计，制备原料包括以下组成：
氧化铝80份、氧化锆12份、氧化铍包覆碳纤维5份、硼砂5份、尿素2.5份。
其中，氧化铍包覆碳纤维的制备方法如下：
将碳纤维预先放入浓硫酸中50℃浸泡30min，滤出水洗至中性后烘干待用，将17.7g BeSO4·4H2O溶于100mL水中，再加入20g经过硫酸处理的碳纤维、450mL环己烷、111.6g吐温-80和65mL正丁醇，高速搅拌后得到微乳液A，将100mL浓氨水、450mL环己烷、111.6g吐温-80和65mL正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌4h后陈化、离心，所得固体依次用水、乙醇、丙酮洗涤后，80℃干燥24h、再转移至马弗炉中以10℃/min的速度升温950℃煅烧3h即可。
上述高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨10h后与氧化铍包覆碳纤维、硼砂、尿素混合均匀，氮气氛围下加热至900℃预烧1h，预烧得到的混合物料再次球磨1h后干燥、造粒，50MPa压制成型得到粗坯，所得粗坯升温至1350℃进行高温烧结，高温烧结时间为2h。
实施例4：
一种高导热氧化铝陶瓷材料，以重量份数计，制备原料包括以下组成：
氧化铝100份、氧化锆12份、氧化铍包覆碳纤维10份、硼砂5份、尿素2.5份。
其中，氧化铍包覆碳纤维的制备方法如下：
将碳纤维预先放入浓硫酸中50℃浸泡30min，滤出水洗至中性后烘干待用，将17.7g BeSO4·4H2O溶于100mL水中，再加入20g经过硫酸处理的碳纤维、450mL环己烷、111.6g吐温-80和65mL正丁醇，高速搅拌后得到微乳液A，将100mL浓氨水、450mL环己烷、111.6g吐温-80和65mL正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌4h后陈化、离心，所得固体依次用水、乙醇、丙酮洗涤后，80℃干燥24h、再转移至马弗炉中以10℃/min的速度升温1000℃煅烧3h即可。
上述高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨10h后与氧化铍包覆碳纤维、硼砂、尿素混合均匀，氮气氛围下加热至1000℃预烧1h，预烧得到的混合物料再次球磨1h后干燥、造粒，50MPa压制成型得到粗坯，所得粗坯升温至1350℃进行高温烧结，高温烧结时间为4h。
实施例5：
一种高导热氧化铝陶瓷材料，以重量份数计，制备原料包括以下组成：
氧化铝80份、氧化锆16份、氧化铍包覆碳纤维5份、硼砂10份、尿素5份。
其中，氧化铍包覆碳纤维的制备方法如下：
将碳纤维预先放入浓硫酸中50℃浸泡30min，滤出水洗至中性后烘干待用，将17.7g BeSO4·4H2O溶于100mL水中，再加入20g经过硫酸处理的碳纤维、450mL环己烷、111.6g吐温-80和65mL正丁醇，高速搅拌后得到微乳液A，将100mL浓氨水、450mL环己烷、111.6g吐温-80和65mL正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌6h后陈化、离心，所得固体依次用水、乙醇、丙酮洗涤后，80℃干燥24h、再转移至马弗炉中以10℃/min的速度升温950℃煅烧5h即可。
上述高导热氧化铝陶瓷材料的制备方法：
将氧化铝、氧化锆混合球磨10h后与氧化铍包覆碳纤维、硼砂、尿素混合均匀，氮气氛围下加热至900℃预烧1h，预烧得到的混合物料再次球磨1h后干燥、造粒，50MPa压制成型得到粗坯，所得粗坯升温至1500℃进行高温烧结，高温烧结时间为1.5h。
对比例1：
与实施例1基本相同，区别在于，不加入氧化铍包覆碳纤维。
对比例2：
与实施例1基本相同，区别在于，用碳纤维代替氧化铍包覆碳纤维。
对比例3：
与实施例1基本相同，区别在于，用氧化铍和碳纤维代替氧化铍包覆碳纤维。
性能测试：
将本发明实施例1-5及对比例1-3中所制备的氧化铝陶瓷材料作为试样；
用WDW-200型电子万能试验机以三点弯曲方式测定试样的抗弯强度(单位：MPa)，加载速度0.5mm/min；跨距16mm，在同一台设备上采用单边切口梁(SENB)法测定试样的断裂韧性(单位：MPa·m1/2)，采用激光导热仪(德国)测试试样的室温热扩散系数，计算得到试样的热导率(单位：W/(m·K))；
测试结果如下表1所示：
表1
| 抗弯强度 | 断裂韧性 | 热导率 | |
| 实施例1 | 586 | 10.7 | 56.2 |
| 实施例2 | 589 | 11.1 | 55.4 |
| 实施例3 | 573 | 9.8 | 54.6 |
| 实施例4 | 578 | 10.4 | 55.8 |
| 实施例5 | 582 | 10.5 | 55.0 |
| 对比例1 | 485 | 7.1 | 20.3 |
| 对比例2 | 550 | 8.6 | 50.2 |
| 对比例3 | 558 | 9.4 | 51.9 |
由上表1可知，本发明所制备的氧化铝陶瓷材料具有良好的导热性能和力学强度，其中，抗弯强度≥573MPa，断裂韧性≥9.8MPa·m1/2，热导率≥54.6W/(m·K)。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种高导热氧化铝陶瓷材料，其特征在于，含有氧化铍包覆一维碳材料。
2.如权利要求1所述的高导热氧化铝陶瓷材料，其特征在于，以重量份数计，制备原料包括以下组成：
氧化铝80-100份、氧化锆12-16份、氧化铍包覆一维碳材料5-10份、硼砂5-10份、尿素1-5份。
3.如权利要求1所述的高导热氧化铝陶瓷材料，其特征在于，所述氧化铍包覆一维碳材料为氧化铍包覆碳纤维或氧化铍包覆碳纳米管。
4.如权利要求1所述的高导热氧化铝陶瓷材料，其特征在于，所述氧化铍包覆一维碳材料的制备方法如下：
将水溶性铍盐溶于水中，再加入一维碳材料、环己烷、吐温-80和正丁醇，高速搅拌后得到微乳液A，将浓氨水、环己烷、吐温-80和正丁醇混合，高速搅拌后得到微乳液B，在搅拌下，将微乳液B滴加入到微乳液A中，搅拌4-6h后陈化、离心，固体洗涤后再经干燥、煅烧即可。
5.如权利要求4所述的高导热氧化铝陶瓷材料，其特征在于，所述一维碳材料预先经过表面粗糙化处理。
6.如权利要求4所述的高导热氧化铝陶瓷材料，其特征在于，所述一维碳材料预先经过浓硫酸浸泡。
7.如权利要求1所述的高导热氧化铝陶瓷材料，其特征在于，煅烧温度为950-1000℃，煅烧时间为3-5h。
8.一种如权利要求1-7中任一项所述的高导热氧化铝陶瓷材料的制备方法，其特征在于，将氧化铝、氧化锆混合球磨后与氧化铍包覆一维碳材料、硼砂、尿素混合加热至900-1000℃进行预烧，得到的混合物料再次球磨后干燥、造粒，压制成型得到粗坯，所得粗坯升温至1350-1500℃进行高温烧结，所述高温烧结时间为1-4h。
9.如权利要求8所述的高导热氧化铝陶瓷材料的制备方法，其特征在于，预烧在氮气氛围下进行。
10.一种陶瓷电路基板，其特征在于，包括如权利要求1-7中任一项所述的高导热氧化铝陶瓷材料。
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