CN102515723A - 细化白色陶瓷材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种细化白色陶瓷材料,属于元器件封装陶瓷材料领域,包括下述重量份的原料:氧化铝87-93份,氧化镁0.8-5份,二氧化硅1-6份,氧化钙0.6-4份,二氧化钛0.01-0.5份,二氧化锆0.5-3份。其制备方法包括:(1)清洗氧化铝磨球和球磨罐,晾干待用;(2)称取0.5-4重量份的溶剂NP-10,并将其加入球磨罐;(3)称取原料,将原料加入球磨罐,球磨72±0.5h。本发明的细化白色陶瓷材料得到的陶瓷晶粒尺寸均匀,表面粗糙度小,瓷体抗断裂性能好。
Description
技术领域
本发明涉及一种陶瓷材料及其制备方法,尤其是一种细化白色陶瓷材料及其制备方法。
背景技术
微电子技术要求其器件封装要有密集、轻薄、快速和散热快的特点。陶瓷封装能满足这些要求,其相对于其它封装形式的优势是其气密性密封性能好,所以被用于高级密封芯片封装,尤其对于军用元器件的封装来说,陶瓷封装的高可靠性是金属封装和塑封无法替代的。
陶瓷材料的力学性能是指在机械力作用下材料发生形变或断裂破坏中所表现的行为特性,主要包括弹性、塑性、断裂性能、蠕变、疲劳和冲击性能等,其中断裂性能是对陶瓷来说最重要的性能。对于大多数无机材料尤其是使用条件复杂的功能无机材料来说,力学性能是工程应用需要首先考虑的因素之一,基体材料力学性能的影响因素及其优化方案设计,对于产品的研制开发及推广应用具有重要意义。
发明内容
本发明提供一种细化白色陶瓷材料及其制备方法,本发明的陶瓷材料得到的陶瓷晶粒尺寸均匀、表面粗糙度小,有较强的抗断裂性能。
本发明所采取的技术方案是:
提供一种细化白色陶瓷材料,包括下述重量份的原料:氧化铝87-93份,氧化镁0.8-5份,二氧化硅1-6份,氧化钙0.6-4份,二氧化钛0.01-0.5份,二氧化锆0.5-3份。
本发明的细化白色陶瓷材料是通过溶剂和原料共球磨的方法制备的。
本发明还提供了细化白色陶瓷材料的制备方法,包括下述步骤:
(1)清洗氧化铝磨球和球磨罐,晾干待用;
(2)称取0.5-4重量份的溶剂NP-10,并将其加入球磨罐;
(3)称取下述重量份的原料:氧化铝87-93份、氧化镁0.8-5份、二氧化硅1-6份、氧化钙0.6-4份、二氧化钛0.01-0.5份和二氧化锆0.5-3份,将原料加入球磨罐,球磨72±0.5h。
其中,步骤(1)中氧化铝磨球和球磨罐的清洗方法为:将氧化铝磨球装入清洗后球磨罐中,向球磨罐中加入无水乙醇至恰能没过氧化铝磨球,封口球磨3h±0.5h。
本发明通过调整配方得到新型陶瓷材料,由于原料中氧化镁、二氧化硅、氧化钙、二氧化钛和二氧化锆的共同作用,在烧结过程中可以有效抑制晶粒的长大。晶粒越细小,材料中晶界比例越大。而事实上,晶界比晶粒内部结合弱,如多晶Al2O3的晶粒内部断裂表面能为46 J/m2,而晶界的表面能γint仅为18 J/m2。但实际上,结合能低的晶界比例越大,材料的强度却越高。这是因为从微观来说,材料的破坏分为沿晶破坏和穿晶破坏,相同的材料成分,发生沿晶破坏时,裂纹扩展要走的道路迂回曲折,晶粒越细,裂纹路径愈长;加之裂纹表面上晶粒的桥接咬合作用还要消耗多余部分能量,故出现晶界越多,强度反而越高的现象。
溶剂NP-10为壬基酚聚氧乙烯(10)醚,混料时加入NP-10作分散剂,能防止被混合粉末发生团聚,起到分散颗粒的作用。
目前电子封装外壳常用白色氧化铝陶瓷主要需要提升材料的断裂强度性能,对于多晶陶瓷材料,断裂强度符合Hall-Petch关系:
σf =σ0+kd 1/2
式中,σ0为无限大单晶的强度;k为系数;d为晶粒直径。
如果起始裂纹受晶粒限制,其尺度将与晶粒度相当,晶粒越细小,初始裂纹尺寸就越小,所以脆性断裂与晶粒度的关系可改写为:
σf =k2d -1/2
断裂强度性能主要取决于材料的化学成分、晶粒尺寸、气孔率、晶体结构类型、微裂纹、玻璃相、表面粗糙度等因素。对于封装陶瓷来说,化学成分受到其功能性限制较多,故晶粒尺寸、晶界相、表面粗糙度等影响因素就成为首要因素。
1.晶粒尺寸
对于多晶陶瓷材料,晶粒越细小,断裂强度越高,这与金属的规律类似。
当晶粒尺寸细小到纳米量级时,材料的强度与晶粒尺寸之间不再一定服从Hall-Petch关系而变得复杂化,因此晶粒尺寸也并非越小越好。
通过查阅文献并结合在本领域内的研究经验表明,晶粒的尺寸分布主要集中于2-3μm,最大晶粒尺寸不超过5μm,无过大或过小晶粒,这种晶粒尺寸的分布情况是较为合理的。
2.晶界相
陶瓷材料在烧结时大都要加入助烧剂,以形成一定量的低熔点相来促进致密化,烧结完毕这些低熔点相便在晶界或角隅处遗留下来形成晶界相。晶界相的成分、性质和数量(厚度)对强度有很大影响。晶界相由于富含杂质或多为非晶态,一般情况下其断裂表面能低、强度低、质脆,故它们的存在对强度不利。
3.表面粗糙度
试样的表面粗糙度会显著影响陶瓷的强度,表面越光滑,缺陷越少、缺陷尺寸越小,强度越高。Griffith对玻璃棒的强度测试发现,刚刚拉制的玻璃棒的弯曲强度(6GPa)明显高于在空气中放置几小时后的强度(0.4GPa),这主要是大气腐蚀形成表面裂纹的缘故。又如,用温水溶去NaCl的表面缺陷后,其强度由5MPa增至1.6GPa。可见,表面缺陷对强度影响之大。
本方法制备得到的陶瓷材料的SEM分析图和原陶瓷SEM分析图分别见图1和图2,由图1和图2可以看到改进后的陶瓷晶粒尺寸均匀,无明显长大晶粒,且晶粒间结合紧密,晶界分布和角度合理。
采用单边切口梁法对本发明陶瓷进行断裂强度测试,并和原陶瓷进行对比,对比图见图3,由图3可以看到本发明的陶瓷强度提高了65%左右,瓷体抗断裂性能有显著提升。
采用上述技术方案所产生的有益效果在于:
1.由于原料中氧化镁、二氧化硅、氧化钙、二氧化钛和二氧化锆的作用,在烧结过程中可以有效抑制晶粒的长大。晶粒越细小,材料中晶界比例越大,结合能低的晶界比例越大,材料的强度就越高。
2.球磨时加入溶剂NP-10,能有效的分散颗粒,防止被混合粉末发生团聚。
3.本发明的陶瓷粉体经烧结后得到的陶瓷表面粗糙度小,表面越光滑,缺陷越少,缺陷尺寸越小,强度越高。
附图说明
下面结合附图和具体实施方式对本发明作进一步详细的说明。
图1是本发明的陶瓷材料的SEM分析图;
图2是原陶瓷材料的SEM分析图;
图3是本发明陶瓷材料和原陶瓷材料的断裂强度测试对比图。
具体实施方式
实施例1
(1)将氧化铝磨球装入球磨罐中,向球磨罐中加入无水乙醇至恰能没过氧化铝磨球,封口球磨3h,倒出乙醇溶液,晾干待用;
(2)称取2重量份的溶剂NP-10,并将其加入球磨罐;
(3)称取下述重量份的原料:氧化铝90份、氧化镁0.8份、二氧化硅6份、氧化钙1.5份、二氧化钛0.01份和二氧化锆2份,将原料加入球磨罐球磨72h。
实施例2
(1)将氧化铝磨球装入球磨罐中,向球磨罐中加入无水乙醇至恰能没过氧化铝磨球,封口球磨3.5h,倒出乙醇溶液,晾干待用;
(2)称取0.5重量份的溶剂NP-10,并将其加入球磨罐;
(3)称取下述重量份的原料:氧化铝87份、氧化镁3份、二氧化硅1份、氧化钙4份、二氧化钛0.25份和二氧化锆3份,将原料加入球磨罐,球磨72.5h。
实施例3
(1)将氧化铝磨球装入球磨罐中,向球磨罐中加入无水乙醇至恰能没过氧化铝磨球,封口球磨2.5h,倒出乙醇溶液,晾干待用;
(2)称取4重量份的溶剂NP-10,并将其加入球磨罐;
(3)称取下述重量份的原料:氧化铝93份、氧化镁5份、二氧化硅2.5份、氧化钙0.6份、二氧化钛0.5份和二氧化锆0.5份,将原料加入球磨罐,球磨71.5h。
Claims (4)
1.一种细化白色陶瓷材料,其特征在于包括下述重量份的原料:氧化铝87-93份,氧化镁0.8-5份,二氧化硅1-6份,氧化钙0.6-4份,二氧化钛0.01-0.5份,二氧化锆0.5-3份。
2.如权利要求1所述的一种细化白色陶瓷材料,其特征在于所述细化白色陶瓷材料是通过溶剂和原料共球磨的方法制备的。
3.一种细化白色陶瓷材料的制备方法,其特征在于包括下述步骤:
(1)清洗氧化铝磨球和球磨罐,晾干待用;
(2)称取0.5-4重量份的溶剂NP-10,并将其加入球磨罐;
(3)称取下述重量份的原料:氧化铝87-93份、氧化镁0.8-5份、二氧化硅1-6份、氧化钙0.6-4份、二氧化钛0.01-0.5份和二氧化锆0.5-3份,将原料加入球磨罐,球磨72±0.5h。
4.如权利要求3所述的一种细化白色陶瓷材料的制备方法,其特征在于步骤(1)中氧化铝磨球和球磨罐的清洗方法为:将氧化铝磨球装入清洗后球磨罐中,向球磨罐中加入无水乙醇至恰能没过氧化铝磨球,封口球磨3h±0.5h。
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