CN110357638A - 一种钛基高导热陶瓷电路基板材料及其制备方法 - Google Patents

一种钛基高导热陶瓷电路基板材料及其制备方法 Download PDF

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CN110357638A
CN110357638A CN201910690121.6A CN201910690121A CN110357638A CN 110357638 A CN110357638 A CN 110357638A CN 201910690121 A CN201910690121 A CN 201910690121A CN 110357638 A CN110357638 A CN 110357638A
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邵伟
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Zhejiang Aixin Electronic Technology Co Ltd
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Abstract

本发明提供了一种钛基高导热陶瓷电路基板材料及其制备方法，其特征在于，由以下重量份的原料制备而成：氮化钛50‑70份、碳化钛45‑60份、氧化铝15‑30份、氮化硅18‑25份、立方氮化硼10‑20份、碳纳米管12‑23份、烧结助剂5‑10份、酚醛树脂6‑12份、聚乙烯醇3‑6份、聚甲基丙烯酸甲酯8‑16份、邻苯二甲酸二丁酯2‑5份、二马来酸二丁基锡4‑8份、3‑巯基丙基三乙氧基硅烷7‑12份、氧化聚乙烯3‑8份、烷基酚聚氧乙烯聚氧丙烯醚2‑6份、N‑甲基吡咯烷酮15‑30份、水20‑40份。本发明制得的陶瓷电路基板材料具有优良的导热性能和力学性能，其作为电路基板材料具有广泛的应用前景。

Description

一种钛基高导热陶瓷电路基板材料及其制备方法
技术领域
本发明属于电子材料技术领域，具体涉及一种钛基高导热陶瓷电路基板材料及其制备方法。
背景技术
随着经济的发展，电子产品如今已经应用于各行各业。目前，我国将智能化制造列入了国家“2016~2020”规划文件中，智能制造的核心是集成电路产品，它包含了成千上万个电子部件。在实际应用中，要让各个电子元器件不相互干扰，必须在集成电路板上使上使用高性能的材料。自20世纪90年代以来，电路基板已经进入了多层基板时代，基板的材质包括无机材料基板、有机材料基板以及复合材料基板。而无机材料基板在导电性能方面具有独特的优势，被世界各国将其用于MCM电路基板行业。导电陶瓷是一种同时具有金属电学特性和陶瓷结构特性于一体的高性能功能材料，由于其在微观结构方面具有陶瓷结构特征，从而使其所制备的产品拥有一般金属材料所不能比拟的物理和化学性能。然而，随着对产品性能要求的不断提高，对电路基板材料的要求越来越高，尤其对于材料的导热性和力学性能，对电路元件的使用性能起到重要的作用。
发明内容
针对以上现有技术存在的问题，本发明的目的在于提供一种钛基高导热陶瓷电路基板材料及其制备方法。
为了实现上述目的，本发明提供以下技术方案：
一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛50-70份、碳化钛45-60份、氧化铝15-30份、氮化硅18-25份、立方氮化硼10-20份、碳纳米管12-23份、烧结助剂5-10份、酚醛树脂6-12份、聚乙烯醇3-6份、聚甲基丙烯酸甲酯8-16份、邻苯二甲酸二丁酯2-5份、二马来酸二丁基锡4-8份、3-巯基丙基三乙氧基硅烷7-12份、氧化聚乙烯3-8 份、烷基酚聚氧乙烯聚氧丙烯醚2-6份、N-甲基吡咯烷酮15-30份、水20-40份。
优选的，本发明所述的一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛60份、碳化钛52份、氧化铝23份、氮化硅21份、立方氮化硼15份、碳纳米管18 份、烧结助剂8份、酚醛树脂9份、聚乙烯醇4.5份、聚甲基丙烯酸甲酯12份、邻苯二甲酸二丁酯3.5份、二马来酸二丁基锡6份、3-巯基丙基三乙氧基硅烷10份、氧化聚乙烯5.5份、烷基酚聚氧乙烯聚氧丙烯醚4份、N-甲基吡咯烷酮23份、水30份。
优选的，所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
优选的，所述的碳纳米管的直径小于10nm。
进一步的，本发明所述的一种钛基高导热陶瓷电路基板材料的制备方法，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理20-40min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散1-2h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为130-150℃，混炼时间为20-40min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
优选的，本发明所述的一种钛基高导热陶瓷电路基板材料的制备方法中，所述步骤(2)中双螺杆挤出机的条件为：挤出温度为160-190℃，螺杆转速为50-70r/min。
优选的，本发明所述的一种钛基高导热陶瓷电路基板材料的制备方法中，所述步骤(3)中排胶的温度为400-600℃。
优选的，本发明所述的一种钛基高导热陶瓷电路基板材料的制备方法中，所述步骤(3)中烧结的条件为：在氮气氛围下以1000-1300℃的温度保温烧结3-6h。
有益效果：本发明提供了一种钛基高导热陶瓷电路基板材料及其制备方法，本发明以氮化钛和碳化钛作为主体材料，辅以氧化铝、氮化硅、立方氮化硼、碳纳米管，从而与主体材料形成特殊的晶体结构，再与烧结助剂以及其他功能原料复配烧结，制备出具有高导热率的陶瓷电路基板材料，同时该基板材料具有优良的力学性能。使用本发明原料制备陶瓷基板材料的过程中，能够提高陶瓷基本的孔隙率和致密度，从而对材料导热性能的提高具有重要的作用。通过测试结果得出，本发明制得的陶瓷电路基板材料的热导率高达172.5W/k.m，弯曲强度高达966.8MPa，断裂韧性高达6.86MPa·m1/2，高的断裂韧性使其具备优良的加工性能。该材料具有优良的导热性能和力学性能，因此其作为电路基板材料具有广泛的应用前景。
具体实施方式
下面结合具体实施例来进一步描述本发明，但实施例仅是范例性的，并不对本发明的范围构成任何限制。本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换，但这些修改和替换均落入本发明的保护范围内。
实施例1
一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛60份、碳化钛 52份、氧化铝23份、氮化硅21份、立方氮化硼15份、碳纳米管18份、烧结助剂8份、酚醛树脂9份、聚乙烯醇4.5份、聚甲基丙烯酸甲酯12份、邻苯二甲酸二丁酯3.5份、二马来酸二丁基锡6份、3-巯基丙基三乙氧基硅烷10份、氧化聚乙烯5.5份、烷基酚聚氧乙烯聚氧丙烯醚4份、N-甲基吡咯烷酮23份、水30份。
所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
所述的碳纳米管的直径小于10nm。
一种钛基高导热陶瓷电路基板材料的制备方法，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理30min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散1.5h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为140℃，混炼时间为30min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
所述步骤(2)中双螺杆挤出机的条件为：挤出温度为175℃，螺杆转速为60r/min。
所述步骤(3)中排胶的温度为500℃。
所述步骤(3)中烧结的条件为：在氮气氛围下以1150℃的温度保温烧结4.5h。
实施例2
一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛50份、碳化钛45份、氧化铝15份、氮化硅18份、立方氮化硼10份、碳纳米管12份、烧结助剂5份、酚醛树脂6份、聚乙烯醇3份、聚甲基丙烯酸甲酯8份、邻苯二甲酸二丁酯2份、二马来酸二丁基锡4份、3-巯基丙基三乙氧基硅烷7份、氧化聚乙烯3份、烷基酚聚氧乙烯聚氧丙烯醚2 份、N-甲基吡咯烷酮15份、水20份。
所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
所述的碳纳米管的直径小于10nm。
一种钛基高导热陶瓷电路基板材料的制备方法，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理20min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散1h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为130℃，混炼时间为20min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
所述步骤(2)中双螺杆挤出机的条件为：挤出温度为160℃，螺杆转速为50r/min。
所述步骤(3)中排胶的温度为400℃。
所述步骤(3)中烧结的条件为：在氮气氛围下以1000℃的温度保温烧结3h。
实施例3
一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛55份、碳化钛 50份、氧化铝20份、氮化硅20份、立方氮化硼12份、碳纳米管15份、烧结助剂6份、酚醛树脂8份、聚乙烯醇4份、聚甲基丙烯酸甲酯10份、3份、二马来酸二丁基锡5份、3-巯基丙基三乙氧基硅烷8份、氧化聚乙烯5份、烷基酚聚氧乙烯聚氧丙烯醚3份、N-甲基吡咯烷酮20份、水25份。
所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
所述的碳纳米管的直径小于10nm。
一种钛基高导热陶瓷电路基板材料的制备方法，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理25min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散1.2h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为135℃，混炼时间为25min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
所述步骤(2)中双螺杆挤出机的条件为：挤出温度为170℃，螺杆转速为55r/min。
所述步骤(3)中排胶的温度为450℃。
所述步骤(3)中烧结的条件为：在氮气氛围下以1100℃的温度保温烧结4h。
实施例4
一种钛基高导热陶瓷电路基板材料，由以下重量份的原料制备而成：氮化钛70份、碳化钛 60份、氧化铝30份、氮化硅25份、立方氮化硼20份、碳纳米管23份、烧结助剂10份、酚醛树脂12份、聚乙烯醇6份、聚甲基丙烯酸甲酯16份、邻苯二甲酸二丁酯5份、二马来酸二丁基锡8份、3-巯基丙基三乙氧基硅烷12份、氧化聚乙烯8份、烷基酚聚氧乙烯聚氧丙烯醚6份、N-甲基吡咯烷酮30份、水40份。
所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
所述的碳纳米管的直径小于10nm。
一种钛基高导热陶瓷电路基板材料的制备方法，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理40min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散2h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为150℃，混炼时间为40min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
所述步骤(2)中双螺杆挤出机的条件为：挤出温度为190℃，螺杆转速为70r/min。
所述步骤(3)中排胶的温度为600℃。
所述步骤(3)中烧结的条件为：在氮气氛围下以1300℃的温度保温烧结6h。
对比例1
对比例1与实施例1的区别在于，对比例1中未添加碳纳米管和立方氮化硼。
对比例2
对比例2与实施例1的区别在于，对比例2中未添加烧结助剂。
将实施例1-4以及对比例1-2制得的陶瓷电路基板材料进行以下性能测试，测试结果如表1 所示，从表1中得出，本发明制得的陶瓷电路基板材料的热导率高达172.5W/k.m，弯曲强度高达966.8MPa，断裂韧性高达6.86MPa·m1/2，因此该材料具有优良的导热性能和力学性能，其作为电路基板材料具有广泛的应用前景。
表1

Claims (8)

1.一种钛基高导热陶瓷电路基板材料，其特征在于，由以下重量份的原料制备而成：氮化钛50-70份、碳化钛45-60份、氧化铝15-30份、氮化硅18-25份、立方氮化硼10-20份、碳纳米管12-23份、烧结助剂5-10份、酚醛树脂6-12份、聚乙烯醇3-6份、聚甲基丙烯酸甲酯8-16份、邻苯二甲酸二丁酯2-5份、二马来酸二丁基锡4-8份、3-巯基丙基三乙氧基硅烷7-12份、氧化聚乙烯3-8份、烷基酚聚氧乙烯聚氧丙烯醚2-6份、N-甲基吡咯烷酮15-30份、水20-40份。
2.根据权利要求1所述的一种钛基高导热陶瓷电路基板材料，其特征在于，由以下重量份的原料制备而成：氮化钛60份、碳化钛52份、氧化铝23份、氮化硅21份、立方氮化硼15份、碳纳米管18份、烧结助剂8份、酚醛树脂9份、聚乙烯醇4.5份、聚甲基丙烯酸甲酯12份、邻苯二甲酸二丁酯3.5份、二马来酸二丁基锡6份、3-巯基丙基三乙氧基硅烷10份、氧化聚乙烯5.5份、烷基酚聚氧乙烯聚氧丙烯醚4份、N-甲基吡咯烷酮23份、水30份。
3.根据权利要求1所述的一种钛基高导热陶瓷电路基板材料，其特征在于，所述的烧结助剂为质量比为1:3:2的MgO、CuO和TiO2。
4.根据权利要求1所述的一种钛基高导热陶瓷电路基板材料，其特征在于，所述的碳纳米管的直径小于10nm。
5.权利要求1-4任一项所述的一种钛基高导热陶瓷电路基板材料的制备方法，其特征在于，包括以下步骤：
(1)将氮化钛、碳化钛、氧化铝、氮化硅、立方氮化硼和碳纳米管置于球磨机中进行球磨处理20-40min，然后加入3-巯基丙基三乙氧基硅烷继续球磨分散1-2h，将混合均匀的原料与剩余原料加入混炼机中进行混炼，制得混炼料；其混炼温度为130-150℃，混炼时间为20-40min，制得混炼料；
(2)将所述混炼料转移至双螺杆挤出机中，熔融挤出造粒，然后放入模具中通过热压成型的方法成型生坯；
(3)将热压成型的生坯进行排胶，去除生坯中的有机互溶剂，再将排胶后的坯件进行烧结，烧结结束后自然冷却至室温，即得所述陶瓷电路基板材料。
6.根据权利要求5所述的一种钛基高导热陶瓷电路基板材料的制备方法，其特征在于，所述步骤(2)中双螺杆挤出机的条件为：挤出温度为160-190℃，螺杆转速为50-70r/min。
7.根据权利要求5所述的一种钛基高导热陶瓷电路基板材料的制备方法，其特征在于，所述步骤(3)中排胶的温度为400-600℃。
8.根据权利要求5所述的一种钛基高导热陶瓷电路基板材料的制备方法，其特征在于，所述步骤(3)中烧结的条件为：在氮气氛围下以1000-1300℃的温度保温烧结3-6h。
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