CN116655399A - 一种氮化铝粉体浆料及其提高封装外壳可靠性的方法 - Google Patents
一种氮化铝粉体浆料及其提高封装外壳可靠性的方法 Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 109
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
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- ZXLATLRDPABPLH-UHFFFAOYSA-N 2-(6-methylheptoxycarbonyl)cyclohexane-1-carboxylic acid Chemical group CC(C)CCCCCOC(=O)C1CCCCC1C(O)=O ZXLATLRDPABPLH-UHFFFAOYSA-N 0.000 claims description 3
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- 238000001465 metallisation Methods 0.000 abstract description 13
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- 229910052573 porcelain Inorganic materials 0.000 abstract 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
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- 238000010344 co-firing Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 229910000833 kovar Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 3
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- MSNOMDLPLDYDME-UHFFFAOYSA-N gold nickel Chemical compound [Ni].[Au] MSNOMDLPLDYDME-UHFFFAOYSA-N 0.000 description 2
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
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- 239000010937 tungsten Substances 0.000 description 2
- 239000004805 Cyclohexane-1,2-dicarboxylic acid Substances 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及陶瓷金属一体化封装技术领域，具体涉及一种氮化铝粉体浆料及其提高封装外壳可靠性的方法。包括制备氮化铝粉体浆料、制备流延浆料、真空脱泡并裁切为生瓷带、利用生瓷带制备封装外壳所需的氮化铝陶瓷、超声酸洗和印制金属化浆料，二次高温烧结固化等步骤，最终形成所需的氮化铝陶瓷金属一体化封装外壳。本发明通过在现有氮化铝粉体浆料中添加一定比例的致孔剂成分，然后在侧印金属化之前通过超声酸洗去除瓷体侧壁中的致孔剂以形成微米级的孔洞，进而大大增强侧印金属化浆料对瓷体的渗透能力，从而改善二者之间的结合力。该方法对封装外壳整体可靠性提升效果明显，方法简单易操作。
Description
技术领域
本发明涉及陶瓷金属一体化封装技术领域，具体涉及一种氮化铝粉体浆料及利用其提高氮化铝陶瓷金属一体化封装外壳可靠性的方法。
背景技术
随着现代电子技术的迅猛发展，电子器件和电路***不断朝着小型化、高功率密度、高频率、高精度方向发展，要求电子封装材料具有更优异的散热性能。其中氮化铝陶瓷作为一种新型功能陶瓷材料，其理论热导率可达320W/m·k，同时具有介电常数和介电损耗极低、绝缘性能良好、与Si、GaAs等半导体材料相匹配的热膨胀系数、力学性能优良、安全无毒等优点。因此氮化铝陶瓷及氮化铝陶瓷金属一体化管壳被广泛的应用于对散热性能或高频性能要求极高的混合集成电路、微波功率器件和光通讯器件封装领域，同时其在医疗、照明、激光打印、航空、通讯、卫星等行业也有着广泛的应用。
目前主流的氮化铝陶瓷金属封装外壳的结构是由可伐环框、氮化铝陶瓷及钨铜底板组成的焊接结构，由于不同材料之间热膨胀系数不一致，在工作时由于温度的交替变化，往往会导致焊缝处产生变化的热应力，导致连接薄弱的界面处产生裂缝，最终造成密封性丧失。其中陶瓷表面的金属化层作为陶瓷与其他金属件焊接的部位其与陶瓷自身之间的结合力对封装外壳整体的可靠性有着至关重要的影响。
氮化铝陶瓷表面金属化层可以分为生瓷阶段印制的表面金属化层及熟瓷阶段印制的侧面金属化层两个部分，由于生瓷阶段印制的金属浆料可以渗透到氮化铝分子的间隙中再经过一起高温共烧形成一种与氮化铝分子互穿的致密型结构，因此这样的金属化层其结合力是相当牢固的。而熟瓷阶段印制的金属化层由于瓷体已经经过高温共烧，其氮化铝分子已经形成致密的晶体结构因此金属化层难以渗透到氮化铝分子间导致这二者之间的结合力相对较为薄弱，而大量的可靠性实验也都表明熟瓷印制的金属化层(侧印金属化层)处容易出现气密性失效问题。因此有必要改善侧印金属化层和陶瓷之间的结合力以提升封装外壳整体的可靠性。
中国专利CN112341250介绍了一种提升氧化锆陶瓷表面金属化层结合力的方法，其主要工艺步骤包括除油(对陶瓷表面进行除油清洗)、粗化(利用氢氟酸、微蚀盐、表面活性剂对陶瓷表面进行蚀刻以生成微小孔洞)、调整(利用调整剂改变陶瓷表面的电性质促进后续胶体钯的吸附)、活化(将胶体钯浸渍吸附到陶瓷表面的孔洞内)、解胶(利用解胶剂将吸附的胶体钯表面的胶体剥离掉以露出钯离子)、化学镀铜(利用钯离子的催化对陶瓷表面进行化学镀铜)、电镀镍金(对化镀铜后的陶瓷表面进行电镀镍金)。整体工艺步骤较为繁琐，且所用到的氢氟酸对操作人员的危害性极大，另外氢氟酸对氧化锆陶瓷表面的刻蚀是各向同性的，因而既要保证粗化效果又要保证瓷体的整体强度，其工艺控制难度非常大。
提供一种工艺简单、无毒无害的改善侧印金属化层和陶瓷之间的结合力以提升封装外壳整体的可靠性的方法是亟需解决的问题。
发明内容
针对现有技术中存在的问题，本发明目的之一在于提供一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法。
本发明采用的技术方案如下：
一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，该方法利用如下步骤制备的氮化铝陶瓷制作氮化铝陶瓷金属一体化封装外壳，步骤为：
S1.制备氮化铝粉体浆料：按所需比例称取氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂，并混合研磨至粒径D50在0.5～1.5μm，得到氮化铝粉体浆料，所述致孔剂为氧化铝粉体；
S2.制备流延浆料：按所需比例称取粘结剂和增塑剂，并与氮化铝粉体浆料混合后继续共同研磨2～4h，得到均匀的流延浆料；
S3.流延浆料进行真空脱泡，脱泡结束后将所述流延浆料流延成型并裁切为生瓷带，并利用所述生瓷带制备封装外壳所需的氮化铝陶瓷；
S4.氮化铝陶瓷经高温共烧后，超声酸洗3～5min，再用纯水清洗干净并烘干；
S5.烘干后的氮化铝陶瓷表面根据需求印制金属化浆料，二次高温烧结固化所述金属化浆料为金属化层，并在所述金属化层外进行镀敷处理，得到所需的氮化铝陶瓷。
优选的，所述溶剂为无水乙醇或丙酮，分散剂为DISPERBYK190，防沉剂为聚烯烃蜡和/或聚酰胺蜡。
优选的，所述氮化铝粉体浆料中，氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂的质量比为(45～60):(35～45):(1～2):(1～2):(1～5)。
优选的，所述步骤S1中制备氮化铝粉体浆料的具体操作为：按所需比例称取氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂，先将防沉剂加入到溶剂中，以1500rpm/min搅拌0.5～1小时，使防沉剂均匀分散到溶剂中，再将含防沉剂的溶剂、氮化铝粉体、分散剂和致孔剂一同加入到研磨机中，混合均匀并研磨形成氮化铝粉体浆料。
优选的，所述粘结剂为聚丙烯酸树脂，所述增塑剂为环己烷-1,2-二羧酸异辛酯。
优选的，所述粘结剂占流延浆料总质量的5～8％，所述增塑剂占流延浆料总质量的1～2％。
优选的，所述步骤S3中，将流延浆料转移至真空搅拌脱泡机中进行真空脱泡，待所述流延浆料的粘度达到3000～6000Pa·S时停止脱泡。
优选的，所述酸洗采用体积浓度为10～50％的稀盐酸，超声频率为20～40KHz。
本发明目的之二在于提供一种氮化铝粉体浆料，该氮化铝粉体浆料用于制备如上所述的方法中的氮化铝陶瓷；该浆料由氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂按质量比(45～60):(35～45):(1～2):(1～2):(1～5)混合组成，所述致孔剂为氧化铝粉体。
优选的，所述氮化铝粉体粒径在0.5～1.5μm，溶剂为无水乙醇或丙酮，分散剂为DISPERBYK190，防沉剂为聚烯烃蜡和/或聚酰胺蜡；所述致孔剂的粒径为0.5～1.5μm。
优选的，还包括粘结剂和增塑剂，所述粘结剂为聚丙烯酸树脂，所述增塑剂为环己烷-1,2-二羧酸异辛酯；所述粘结剂占流延浆料的质量比为5～8％，所述增塑剂占流延浆料的质量比为1～2％。
本发明还提供一种按照上述提高氮化铝陶瓷金属一体化封装外壳可靠性的方法中步骤生产制备的氮化铝陶瓷。
本发明的有益效果在于：
本发明通过在现有氮化铝粉体浆料中添加一定比例的致孔剂成分，致孔剂中的一部分会在高温共烧过程中生成液相促进氮化铝陶瓷的烧结，另一部分则会在高温共烧过程中发生微相分离，然后在侧印金属化之前通过超声酸洗去除瓷体侧壁中的致孔剂以形成微米级的孔洞，进而大大增强侧印金属化浆料对瓷体的渗透能力，从而改善二者之间的结合力。该方法对封装外壳整体可靠性提升效果明显，方法简单易操作。
本发明中致孔剂为氮化铝，通过稀盐酸超声酸洗即可在氮化铝陶瓷表面形成微孔进而增强侧印金属化浆料对瓷体的附着力，本方法不涉及腐蚀性极强的氢氟酸，且超声酸洗仅会和陶瓷侧壁中的致孔剂反应，对瓷体其余位置无腐蚀作用，因而工艺控制难度小，易于操作。另外，本申请方法能够用于氮化铝多层陶瓷的制备工艺中，氮化铝陶瓷相比于氧化锆陶瓷也可以应用到高导热的封装管壳中，提高此两者的封装可靠性。
具体实施方式
下面结合实施例对本发明进行进一步详细说明。
实施例1
一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，首先制备氮化铝陶瓷：
S1.制备氮化铝粉体浆料：按质量份称取55份氮化铝粉体，40份丙酮作为溶剂，1份含颜料亲和基团的高分子量嵌段共聚物溶液DISPERBYK190(德国毕克)作为分散剂，1份聚烯烃蜡作为防沉剂和3份氧化铝粉体作为致孔剂。
先将聚烯烃蜡加入到丙酮中，在高速分散机中以1500rpm/min搅拌45分钟，使聚烯烃蜡均匀分散到丙酮中，再将含聚烯烃蜡的丙酮、DISPERBYK190、氮化铝粉体和氧化铝粉体一同加入到纳米研磨机中，混合均匀并形成氮化铝粉体浆料；
上述氮化铝粉体和氧化铝粉体的粒径均为0.5～1.5μm，若原料未达到该粒度，可在研磨机中按照研磨球与氮化铝粉体的质量比5:1的比例进行研磨，研磨至D50范围在0.5～1.5μm时，停机。
S2.制备流延浆料：按照占氮化铝流延浆料质量比5％称取聚丙烯酸树脂作粘结剂、按占流延浆料质量比1％称取环己烷-1,2-二羧酸异辛酯作增塑剂，然后加入到氮化铝粉体浆料中，共同研磨2～4h后停机，得到混合均匀的流延浆料。
S3.将二次研磨后的流延浆料转移至真空搅拌脱泡机中进行真空脱泡，真空脱泡时间为0.5小时，当流延浆料粘度达到3000～6000Pa·S时停止脱泡。脱泡结束后将所述流延浆料流延成型并裁切为生瓷带，并利用所述生瓷带制备封装外壳所需的氮化铝陶瓷。
上述裁切生瓷带以及制备氮化铝陶瓷的方法均可以根据需求参考现有技术，在一种实施方式中，具体操作步骤如下：
S31.将真空脱泡后的流延浆料转移至流延机进行流延操作，流延速度为0.2～0.5m/min，使流延出的生瓷带厚度控制在0.05～1mm范围内，然后将流延成型的生瓷带裁切为所需尺寸的生瓷片；
S32.对生瓷片进行冲孔并在孔内填充导电浆料，导电浆料选择常规的钨浆料；
S33.在生瓷片表面进行金属浆料的丝网印制以形成内部线路，金属浆料和导电浆料成分一致；
S34.冲空腔，采用常规的激光切割工艺冲空腔；
S35.叠压生瓷片，采用常规的等静压工艺叠压生瓷片；
S36.将叠压生瓷片分切成单独小陶瓷，采用常规的钨钢切刀裁切成单独小陶瓷；
S37.排胶，采用常规高温850℃对单独小陶瓷排胶24～48小时；
S38.高温共烧陶瓷，采用常规高温1800℃共烧24小时，其中一部分氧化铝会形成液相并促进氮化铝晶体的烧结，而至少一部分氧化铝会发生微相分离并形成微米级的团状颗粒，烧结后得到所需的氮化铝陶瓷。
S4.氮化铝陶瓷经高温共烧后，超声酸洗3～5min，其中酸为稀盐酸，其体积浓度为50％，超声时间为5min，超声频率为20～40KHZ；酸洗过程中氮化铝陶瓷瓷体侧壁中团状的致孔剂会与酸发生反应并溶解，最后再用纯水反复清洗至干净并烘干，这样氮化铝陶瓷瓷体侧壁中就形成了密集分布的微米级孔洞。
S5.烘干后的氮化铝陶瓷表面根据需求印制金属化浆料，金属浆料成分和前述生瓷浆料一致；二次高温烧结固化所述金属化浆料为金属化层后，并在所述金属化层外进行镀敷处理，得到所需的氮化铝陶瓷。由于陶瓷中存在微米级的孔洞，大大增强了侧印金属化浆料对瓷体的渗透能力，从而改善了二者之间的结合力。
上述二次高温烧结固化采用常规高温1750℃保温4小时后烧。镀敷处理为电镀镍，镍层厚度2-4μm。
上述S5得到的氮化铝陶瓷与可伐环框、钨铜底板进行银铜共晶钎焊即可得到最终可靠性提高的氮化铝陶瓷金属一体化封装外壳，实际使用中，可根据需求选择不同的封装形式或材质，本发明对此不做具体限定。
实施例2
在实施例1的基础上，调整步骤S1中氮化铝粉体为54份，3份氧化铝粉体为4份氧化镁粉体，制备氮化铝陶瓷。
实施例3
将实施例1和实施例2制备的氮化铝陶瓷分别与可伐引线银铜焊接形成引线陶瓷组件，再将引线陶瓷组件与钨铜底板(W90Cu10)、可伐环框(4J29)进行一体银铜共晶钎焊(Ag72Cu28)得到氮化铝陶瓷金属一体化封装外壳。
上述氮化铝陶瓷金属一体化封装外壳与采用常规方法制备的氮化铝陶瓷条制成的外壳(浆料不包含致孔剂材料，侧印金属化前无酸洗等步骤，其余材料及制备工艺与实施例1完全相同)进行比较，相关性能参数及可靠性测试结果参见下表1：
表1：本发明实施例对比常规方法氮化铝陶瓷外壳性能及可靠性结果
可以看出，本发明方法制备的氮化铝陶瓷应用于封装外壳制备中，在气密性等方面达到标准的情况下，能够降低封装外壳使用中的漏气概率，提高封装可靠性。
以上仅为本发明的较佳实用例而已，并不用以限制本发明创造；尽管参照前述实施方式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：凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明创造的保护范围之内。
Claims (11)
1.一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，该方法利用如下步骤制备的氮化铝陶瓷制作氮化铝陶瓷金属一体化封装外壳，步骤为：
S1.制备氮化铝粉体浆料：按所需比例称取氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂，并混合研磨至粒径D50在0.5～1.5μm，得到氮化铝粉体浆料，所述致孔剂为氧化铝粉体；
S2.制备流延浆料：按所需比例称取粘结剂和增塑剂，并与氮化铝粉体浆料混合后继续共同研磨2～4h，得到均匀的流延浆料；
S3.流延浆料进行真空脱泡，脱泡结束后将所述流延浆料流延成型并裁切为生瓷带，并利用所述生瓷带制备封装外壳所需的氮化铝陶瓷；
S4.氮化铝陶瓷经高温共烧后，超声酸洗3～5min，再用纯水清洗干净并烘干；
S5.烘干后的氮化铝陶瓷表面根据需求印制金属化浆料，二次高温烧结固化所述金属化浆料为金属化层，并在所述金属化层外进行镀敷处理，得到所需的氮化铝陶瓷。
2.如权利要求1所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述溶剂为无水乙醇或丙酮，分散剂为DISPERBYK190，防沉剂为聚烯烃蜡和/或聚酰胺蜡。
3.如权利要求2所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述氮化铝粉体浆料中，氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂的质量比为(45～60):(35～45):(1～2):(1～2):(1～5)。
4.如权利要求1-3任一项所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述步骤S1中制备氮化铝粉体浆料的具体操作为：按所需比例称取氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂，先将防沉剂加入到溶剂中，以1500rpm/min搅拌0.5～1小时，使防沉剂均匀分散到溶剂中，再将含防沉剂的溶剂、氮化铝粉体、分散剂和致孔剂一同加入到研磨机中，混合均匀并研磨形成氮化铝粉体浆料。
5.如权利要求1-3任一项所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述粘结剂为聚丙烯酸树脂，所述增塑剂为环己烷-1,2-二羧酸异辛酯。
6.如权利要求5所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述粘结剂占流延浆料总质量的5～8％，所述增塑剂占流延浆料总质量的1～2％。
7.如权利要求1所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述步骤S3中，将流延浆料转移至真空搅拌脱泡机中进行真空脱泡，待所述流延浆料的粘度达到3000～6000Pa·S时停止脱泡。
8.如权利要求1所述的一种提高氮化铝陶瓷金属一体化封装外壳可靠性的方法，其特征在于，所述酸洗采用体积浓度为10～50％的稀盐酸，超声频率为20～40KHz。
9.一种氮化铝粉体浆料，其特征在于，用于制备如权利要求1所述的方法中的氮化铝陶瓷；该浆料由氮化铝粉体、溶剂、分散剂、防沉剂和致孔剂按质量比(45～60):(35～45):(1～2):(1～2):(1～5)混合组成，所述致孔剂为氧化铝粉体。
10.如权利要求9所述的一种氮化铝粉体浆料，其特征在于，所述氮化铝粉体粒径在0.5～1.5μm，溶剂为无水乙醇或丙酮，分散剂为DISPERBYK190，防沉剂为聚烯烃蜡和/或聚酰胺蜡；所述致孔剂的粒径为0.5～1.5μm。
11.如权利要求9或10所述的一种氮化铝粉体浆料，其特征在于，还包括粘结剂和增塑剂，所述粘结剂为聚丙烯酸树脂，所述增塑剂为环己烷-1,2-二羧酸异辛酯；所述粘结剂占流延浆料的质量比为5～8％，所述增塑剂占流延浆料的质量比为1～2％。
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