CN115521731A - 一种高导热、低机械加工磨损性的功能填料及其制备方法 - Google Patents
一种高导热、低机械加工磨损性的功能填料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 claims abstract description 19
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- -1 zinc aluminate Chemical class 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 239000011701 zinc Substances 0.000 claims abstract description 14
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 11
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 7
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 7
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- 238000011049 filling Methods 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 6
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- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000000956 alloy Substances 0.000 abstract 1
- HUIAGCXKFBECLZ-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[AlH3].[Zn] HUIAGCXKFBECLZ-UHFFFAOYSA-N 0.000 abstract 1
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Abstract
本发明公开了一种低机械加工磨损性、高导热系数的覆铜板用功能填充料及其制备方法，属于新材料技术领域，该功能填充料为氧化铝和铝酸锌的固溶体，其化学组分为氧化铝占20wt％‑40wt％，铝酸锌占60wt％‑80wt％，其平均粒径为1‑10微米。它是将铝源和锌源混合均匀，并添加一定的助剂，高温煅烧，然后冷却处理，经粉碎、磨细、分级处理即得。该功能填充料硬度适当、导热系数高，适合做高导热、低机械加工磨损性的覆铜板用填充材料，主要应用于覆铜板方面。
Description
技术领域
本发明属于新材料技术领域，具体涉及一种高导热、低机械加工磨损性的功能填料及其制备方法。
背景技术
印制线路板(Printed Circuit Board，简称PCB)是电子信息装备的重要部件。随着电子行业的进步，PCB的基板材料覆铜板(Copper Clad Laminate，简称CCL)如今正在快速的向着更高性能发展。覆铜板作为印制电路板的基体材料起到的作用主要有：导电、导热、绝缘和支撑。
电子产品的发展方向是小型化、高度集成化，相应的覆铜板的轻薄化也是发展方向。覆铜板轻薄化过程中，基板会因厚度降低而刚性同时被削弱，而可能会导致印制线路板制造过程中的操作性变差，制出的印制线路板在回流焊、波峰焊中容易产生翘曲。在提高覆铜板的刚性方面，加入填充料是一种有成效的、较低成本的措施。
另外，电子产品的小型化也使得功率密度越来越大，对覆铜板的导热性要求也越来越高。高度集成化也导致钻孔数量越来越多，钻孔精度和孔壁质量要求越来越高，降低覆铜板的机械加工磨损性的要求也越来越高。
因此，覆铜板中的填充料(Fillers)使用技术已成为覆铜板技术开发中的重要环节。导热覆铜板中使用的填料有氢氧化铝、氧化铝和氧化锌。但氢氧化铝在200多摄氏度就开始分解，不耐热冲击。氧化铝虽然具有很好的化学稳定性和导热率、但由于其莫氏硬度大于9，在覆铜板的钻孔加工过程中对加工钻头的磨损非常严重、大幅增加了加工难度和成本。氧化锌的莫氏硬度小于氧化铝，但其的耐酸、耐化学腐蚀性不够理想，在覆铜板的后处理加工时会增加加工序、致使成本上涨。因此急需开发一种高导热、低机械加工磨损性的覆铜板填料。
发明内容
本发明要解决的技术问题是针对现有技术的不足而提供一种低机械加工磨损性、高导热系数覆铜板用功能填充料及其制备方法。该功能填充料硬度低、导热系数高，适于作覆铜板用填充材料。
为了解决上述技术问题，本发明所采用的技术方案是：
一种低机械磨损性、高导热系数的覆铜板用功能填充料，其特征在于：是氧化铝与铝酸锌的固溶体，其化学组分为氧化铝占20wt％-40wt％，铝酸锌占60wt％-80wt％，平均粒径为1-10微米。由以下步骤制备：
1)原料混合，按重量份数计为：γ氧化铝100份、氧化锌35-55份、硼酸0.5-5份、氟化铝0.5-5份，取上述原料在球磨机中研磨5-10h混匀备用；
2)将步骤1)混匀后的材料在1200℃～1600℃高温煅烧10-30h，形成氧化铝和铝酸锌的固溶体，然后待温度下降，取出并冷却处理，再经破碎、磨细、分级处理而得到氧化铝与铝酸锌的固溶体，其化学组分为氧化铝占20wt％-40wt％，铝酸锌占60wt％-80wt％，平均粒径为1-10微米。氧化铝和氧化锌在硼酸和氟化铝的作用下煅烧生成铝酸锌，氟化铝是矿化剂，硼酸是性能调节剂。氟元素会在煅烧过程挥发，硼酸部分挥发，少量残留在固溶体中可调节晶粒大小。
本发明的有益效果是：通过本发明制备的功能填充料具有良好的低机械加工磨损性，且具有高的导热系数。因此其作为覆铜板填充料，可改善覆铜板的各项性能，具有优异的高导热性能和易加工性。能够有效改善覆铜板钻孔加工工艺，延长钻头的使用寿命，适于全面推广和应用。
具体实施方式
以下结合具体实例对发明的发明内容进行进一步说明：
实施例1：
步骤1：功能填充料制备，按重量份数计为：γ-氧化铝100份、氧化锌35份、硼酸1份、氟化铝2份，称取原料，使用球磨机研磨5-10h混匀备用；在1450℃高温煅烧10-30h形成固溶体，然后待温度下降，取出并冷却，再经破碎、磨细、分级处理即得平均粒径为1-10微米的功能填充材料1。
步骤2：在带搅拌桨的1L烧瓶中加入液体PI树脂150g，然后加入20gDMF(N，N-二甲基甲酰胺)，搅拌约半个小时。然后在另一1L干洁烧瓶中加入350g步骤1合成的功能填充料1，加入130gDMF，将该填料搅拌半个小时混匀。再将混好的树脂倒入该填料中，搅拌一个小时，加入催化剂0.05g。用砂磨机研磨5h，即得上胶所用胶水。采用1080布进行上胶，在155℃下烘3分钟左右得到半固化状态的粘结片。将5张粘结片叠在一起，两面覆上铜箔，于真空压机中200℃，150分钟层压得到导热覆铜箔层压板。用0.3mm钻头进行钻孔，钻速110krpm，落速33mm/s，连续钻5000孔，观察钻头的刃尖磨损情况，由磨损的大小确定钻孔加工性好坏。其他板材性能及见表1。
实施例2：
步骤1：功能填充料制备，按重量份数计为：γ-氧化铝100份、氧化锌45份、硼酸1份、氟化铝2份，称取原料，球磨研磨5-10h混匀备用；在1450℃高温煅烧10-30h，然后待温度下降，取出并冷却，再经破碎、磨细、分级处理即得平均粒径为1-10微米的功能填充材料2。
步骤2：在带搅拌桨的1L烧瓶中加入液体PI树脂150g，然后加入20gDMF(N，N-二甲基甲酰胺)，搅拌约半个小时。然后在另一1L干洁烧瓶中加入350g步骤1合成的功能填充料2，加入130gDMF，将该填料搅拌半个小时，直到填料在溶剂中呈均一状态。再将混好的树脂倒入该填料中，搅拌一个小时，加入催化剂0.05g。用球磨机球磨5h，即得上胶所用胶水。采用1080布进行上胶，在155℃下烘3分钟左右得到半固化状态的粘结片。将5张粘结片叠在一起，两面覆上铜箔，于真空压机中200℃，150分钟层压得到导热覆铜箔层压板。用0.3mm钻头进行钻孔，钻速110krpm，落速33mm/s，连续钻5000孔，观察钻头的刃尖磨损情况，由磨损的大小确定钻孔加工性好坏。其他板材性能及见表1。
实施例3：
步骤1功能填充料制备，按重量份数计为：γ-氧化铝100份、氧化锌55份、硼酸1份、氟化铝2份，称取原料，球磨机研磨5-10h混匀备用；在1450℃高温煅烧10-30h，然后待温度下降，取出并冷却，再经破碎、磨细、分级处理即得平均粒径为1-10微米的功能填充材料3。
步骤2：在带搅拌桨的1L烧瓶中加入液体PI树脂150g，然后加入20gDMF(N，N-二甲基甲酰胺)，搅拌约半个小时。然后在另一1L干洁烧瓶中加入350g步骤1合成的功能填充料3，加入130gDMF，将该填料搅拌半个小时混匀。再将混好的树脂倒入该填料中，搅拌一个小时，加入催化剂0.05g。用砂磨机研磨5h，即得上胶所用胶水。采用1080布进行上胶，在155℃下烘3分钟左右得到半固化状态的粘结片。将5张粘结片叠在一起，两面覆上铜箔，于真空压机中200℃，150分钟层压得到导热覆铜箔层压板。用0.3mm钻头进行钻孔，钻速110krpm，落速33mm/s，连续钻5000孔，观察钻头的刃尖磨损情况，由磨损的大小确定钻孔加工性好坏。其他板材性能及见表1。
比较例1
在带搅拌桨的1L烧瓶中加入液体PI树脂100g，然后加入20gDMF(N，N-二甲基甲酰胺)，搅拌约半个小时。然后在另一1L干洁烧瓶中加入350g5微米球形氧化铝，加入130gDMF，将该填料搅拌半个小时混匀。再将混好的树脂倒入该填料中，搅拌一个小时，加入催化剂0.05g。用砂磨机研磨5h，即得上胶所用胶水。采用1080布进行上胶，在155℃下烘3分钟左右得到半固化状态的粘结片。将5张粘结片叠在一起，两面覆上铜箔，于真空压机中200℃，150分钟层压得到导热覆铜箔层压板。用0.3mm钻头进行钻孔，钻速110krpm，落速33mm/s，连续钻5000孔，观察钻头的刃尖磨损情况，由磨损的大小确定钻孔加工性好坏。其他板材性能及见表1。
比较例2
在带搅拌桨的1L烧瓶中加入液体PI树脂100g，然后加入20gDMF(N，N-二甲基甲酰胺)，搅拌约半个小时。然后在另一1L干洁烧瓶中加入350g氢氧化铝，加入130gDMF，将该填料搅拌半个小时混匀。再将混好的树脂倒入该填料中，搅拌一个小时，加入催化剂0.05g。用砂磨机研磨5h，即得上胶所用胶水。采用1080布进行上胶，在155℃下烘3分钟左右得到半固化状态的粘结片。将5张粘结片叠在一起，两面覆上铜箔，于真空压机中200℃，150分钟层压得到导热覆铜箔层压板。用0.3mm钻头进行钻孔，钻速110krpm，落速33mm/s，连续钻5000孔，观察钻头的刃尖磨损情况，由磨损的大小确定钻孔加工性好坏。其他板材性能及见表1。
表1
由本发明的实施例可以看出，采用由本发明的填料体系制得的覆铜板，不仅具有良好的热导率，而且对钻头的磨损也比单纯的氧化铝填料体系小。对比氢氧化铝填料制得的覆铜板，本发明的填料体系制得的覆铜板具有较高的导热系数。综上所述，本发明提供的导热填料不仅具有良好的导热率并且制作工艺简单、成本低、适合于工业生产。
以上实施方式仅用于说明本发明，而并非对本发明的限制，有关技术领域的普通技术人员，在不脱离本发明的精神和范围的情况下，还可以做出各种变化和变型，因此所有等同的技术方案也属于本发明的范畴，本发明的专利保护范围应由权利要求限定。
Claims (2)
1.一种低机械磨损性、高导热系数的覆铜板用功能填充料，其特征在于：是氧化铝与铝酸锌的固溶体，其化学组分为氧化铝占20wt％-40wt％，铝酸锌占60wt％-80wt％，平均粒径为1-10微米。
2.根据权利要求1所述的一种低机械磨损性、高导热系数的覆铜板用功能填充料的制备方法，其特征在于，由以下步骤制备：
1)原料混合，按重量份数计为：γ氧化铝100份、氧化锌35-55份、硼酸0.5-5份、氟化铝0.5-5份，取上述原料在球磨机中研磨5-10h混匀备用；
2)将步骤1)混匀后的材料在1200℃～1600℃高温煅烧10-30h，形成氧化铝和铝酸锌的固溶体，然后待温度下降，取出并冷却处理，再经破碎、磨细、分级处理而得到氧化铝与铝酸锌的固溶体，其化学组分为氧化铝占20wt％-40wt％，铝酸锌占60wt％-80wt％，平均粒径为1-10微米。
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