CN104080829B - 耐冲击性优秀的热固性环氧树脂组合物 - Google Patents
耐冲击性优秀的热固性环氧树脂组合物 Download PDFInfo
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Abstract
本发明涉及用作半导体封装件等电子材料密封剂的环氧树脂组合物,本发明的热固性环氧树脂组合物包含:环氧树脂,分子内具有两个以上的环氧基;固化剂,包含由化学式1表示的高分子量的聚硫代化合物和由化学式2表示的低分子量的聚硫代化合物的混合物;以及固化促进剂。
Description
技术领域
本发明涉及用作半导体封装件等电子材料密封剂的环氧树脂组合物,更详细地,涉及包含高分子量的聚硫代化合物作为环氧树脂的固化剂的环氧树脂组合物。
背景技术
随着手机之类的电子产品越来越小型化、薄型化,使用于这些电子产品的半导体封装件也主要使用球栅阵列(BGA,BallGridArray)或芯片尺寸封装件(CSP,ChipScalePackage)等的高密度封装件。
如图1所示,球栅陈列封装件10包括:基板12;半导体芯片11,通过引线键合(WireBonding)、倒装芯片(Flipchip)等方法安装(mount)于基板12的上部;以及成形部13,用于保护半导体芯片11。并且,基板12的下部附着与半导体芯片11进行电连接的多个焊球14。具有这种结构的球栅陈列封装件10安装于形成回路图案的配线基板20的表面。但是,构成球栅陈列封装件10的基板12、焊球14及配线基板20等的热膨胀系数互不相同,因而在经由热循环的过程中,因热应力而产生连接不良,因此,在安装球栅陈列封装件10之后,会进行使密封剂30向球栅车裂封装件10和配线基板20之间渗透、固化,来密封上述球栅陈列封装件10和配线基板20的缝隙的底部填充(underfill)工序。
上述密封剂30起到如下作用,即,使上述的热应力得到缓冲,来提高电连接的可靠性,并且,提高连接力,来提高对冲击的耐久性。
因此,密封剂30应在短时间内能够进行固化(固着),且不会对配线基板20或周边部件产生坏影响。并且,应对热循环的耐热冲击性优秀,并且,当产生降落、弯曲等冲击时,可以防止球栅陈列或芯片尺寸封装件脱落。并且,在结束底部填充工序之后,发现半导体芯片11的不良或与配线基板20之间的连接不良等时,应对需要替换球栅陈列封装件或芯片尺寸封装件的情况,可从配线基板20容易分离的重操作性(修复性)应优秀。
作为这种密封剂30主要使用热固性树脂组合物。但是,若使用普通的热固性树脂,则存在以剥离的方式替换球栅陈列封装件或芯片尺寸封装件非常困难的问题。并且,虽然也有使用光固化性粘结剂的情况,但这存在为了使用光固化性粘结剂而需要将配线基板20限定为能够进行光照射的玻璃等透明基板的问题。并且,为了从配线基板20剥离固化性树脂而考虑浸渍于有机溶剂等来进行剥离的方法,但该过程存在用于电连接的粘结性或耐久性反而低下的问题。
日本特许公开平6-77264号提示了代替基于使用溶剂的溶胀或溶解的剥离,以照射电磁波的方式去除剩余树脂的方法。但这种方法不仅需要大规模的设备,而且难以去除剩余的粘结剂,因此难以视为大幅提高粘结剂的重操作性。
作为应对这些多种问题的方式,最普遍使用的就是环氧树脂组合物。
日本特许公开平10-204259号公开了底部填充用固化性树脂组合物,上述底部填充用固化性树脂组合物在作为赋予重操作性(修复性)的粘结剂的单组分或双组分环氧树脂中添加增塑剂,从而能够进行短时间的热固化,耐热冲击性(温度循环性)优秀,并且,当发现不良时,能够容易地剥离球栅陈列封装件或芯片尺寸封装件。但这由于使用增塑剂,因而存在不仅使树脂的物性,即,耐热冲击性低下,而且使降落冲击性、冲击弯曲性及耐久性等低下,或者在固化物中增塑剂渗漏,从而污染周边的问题。
韩国公开特许第10-2000-0070203号提示了包含双酚A型环氧树脂、固化剂及增塑剂的热固性树脂组合物,韩国公开特许第10-2001-0102206号提示了包含多官能性环氧树脂(双酚A型环氧树脂等)、固化剂及改性环氧树脂的环氧树脂组合物。此时,固化剂使用胺化合物(双氰胺)、改性胺化合物、咪唑化合物及改性咪唑化合物等。
韩国公开特许第10-2009-0052961号以在双酚型环氧树脂中附加聚硫代树脂的改性环氧树脂作为技术要旨,作为固化剂,使用三羟甲基丙烷三(3-巯基丙酸酯)(TPMP)之类的通用的硫醇化合物。
日本公开特许平6-211970号公开了具有两个以上的硫醇基的聚硫醇化合物,三羟甲基丙烷三硫代巯基丙酸酯[TMTG]=(TMPMP)、三羟甲基丙烷三硫代乙醇酸酯[PETG]=(TMPMA)、季戊四醇四硫代乙醇酸酯[PETG]=(PETMA)及季戊四醇四硫代丙酸酯[PETP]=(PETMP)。
最近,随着电子产品的小型化、集成化倾向,回路配线的间隙或焊球的直径越来越细小,由此,产品的耐热冲击性、降落冲击性及重操作性之类的要求物性基准越来越严格,因此,需要开发能满足一切物性的已提高的环氧树脂组合物。
发明内容
技术问题
本发明用于解决上述的问题,本发明的目的在于,提供使用特定分子量的二成份类聚硫代固化剂,耐热冲击性、降落冲击性及重操作性(修复性)等优秀的环氧树脂组合物和包含该环氧树脂组合物的密封剂。
并且,本发明的目的在于,提供能够满足随着电子产品的小型化、集成化倾向而越来越严格的要求物性基准的环氧树脂组合物。
解决问题的手段
本发明的热固性环氧树脂组合物包含分子内具有两个以上的环氧基的环氧树脂、环氧树脂固化剂及固化促进剂,
相对于100重量份的环氧树脂,上述环氧树脂固化剂包含:
a)40~100重量份的由以下化学式1表示的高分子量的聚硫代化合物,以及
b)20~60重量份的由以下化学式2表示的低分子量的聚硫代化合物。
化学式1:
(在上述化学式中,R为氢、甲基或乙基,x、y、z为0或整数,x、y、z之和为7~25。)
化学式2:
(在上述化学式中,R为氢、甲基或乙基,m为0~2,n为2~4整数,m、n之和为4。)
发明的效果
根据本发明,通过包含化学式1的高分子量的聚硫代化合物和化学式2的低分子量的聚硫代化合物的二成份类聚硫代化合物作为环氧树脂固化剂,具有耐热冲击性、降落冲击性及重操作性(修复性)等优秀的效果。因此,能够满足随着电子产品的小型化、集成化倾向而越来越严格的最近的要求物性基准。并且,根据本发明,由于可以在短时间内进行热固化而提高生产率,且在配线基板确实安装球栅陈列封装件或芯片尺寸封装件等的半导体部件,因而提高产品的可靠性。
附图说明
图1为表示在配线基板上安装球栅阵列封装件的状态的剖视图。
附图标记的说明
10:球栅阵列封装件11:半导体芯片
12:基板13:成形部
14:焊球20:配线基板
30:密封剂
具体实施方式
本发明人员对利用于半导体封装件的环氧树脂组合物进行不断研究的结果,确认了若将由延伸7~25个乙氧基(-CH2CH2O-)的高分子量的巯基丙酸酯类化合物和没有乙氧基的低分子量的巯基丙酸酯类化合物组成的二成份类化合物利用为环氧树脂的固化剂,则提高所固化的环氧树脂的耐热冲击性、降落冲击性及重操作性,从而实现了本发明。
以下,对本发明的优选实施例进行更加详细的说明。
本发明的作为环氧树脂组合物的热固性环氧树脂组合物包含分子内具有两个以上的环氧基的环氧树脂、环氧树脂固化剂及固化促进剂,
相对于100重量份的环氧树脂,上述环氧树脂固化剂包含:
a)40~100重量份的由以下化学式1表示的高分子量的聚硫代化合物,以及
b)20~60重量份的由以下化学式2表示的低分子量的聚硫代化合物。
化学式1:
(在上述化学式中,R为氢、甲基或乙基,x、y、z为0或整数,x、y、z之和为7~250)。
化学式2:
(在上述化学式中,R为氢、甲基或乙基,m为0~2,n为2~4整数,m、n之和为4)。
上述环氧树脂可使用分子内具有两个以上的环氧基的多官能性环氧树脂。例如,可以利用选自包含双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、苯酚酚醛型环氧树脂及甲酚酚醛型环氧树脂等的组中的一种以上的多官能性环氧树脂,但并不局限于此。
并且,根据需要,上述环氧树脂可以包含分子内具有一个环氧基的单官能性环氧树脂作为反应性稀释剂。优选地,这种单官能性环氧树脂具有C6~C28的烷基(AlkylGroup),作为具体例,可使用选自包含C6~C28烷基缩水甘油醚、C6~C28烷基缩水甘油酯及C6~C28苯酚甘油醚等的组中的一种以上,但并不局限于此。优选地,以100重量份的整个环氧树脂为基准,包含0~40重量份的上述单官能性环氧树脂。若单官能性环氧树脂大于40重量份,则可能因接合强度的低下而使可靠性变差。
并且,环氧树脂还可以包含改性环氧树脂。例如,可以为选自包含橡胶改性环氧树脂、氨基甲酸乙酯改性环氧树脂、由大豆油及蓖麻油等植物油改性的环氧树脂、二聚酸改性环氧树脂及丙烯酸改性环氧树脂等的组中的一种以上。
尤其,优选地,环氧树脂包含环氧当量为170~210的双酚A型环氧树脂,分子量优选为340~450g/mol。
本发明的环氧树脂固化剂包含由以下化学式1表示的附加乙氧基的巯基丙酸酯类化合物和由以下化学式2表示的没有乙氧基的巯基丙酸酯类化合物。
化学式1:
(在上述化学式中,R为氢、甲基或乙基,x、y、z为0或整数,x、y、z之和为7~25)。
化学式2:
(在上述化学式中,R为氢、甲基或乙基,m为0~2,n为2~4整数,m、n之和为4)。
在上述化学式1中,乙氧基在分子内由7~25个组成,优选地,由7~20个组成。上述聚硫代化合物为在以往用作环氧树脂固化剂的巯基丙酸酯类化合物附加多个乙氧基而成,通过将分子的链长度变长,使得环氧树脂之间的键合变得稍微灵活,从而使降落冲击性显著提高。若没有乙氧基或乙氧基在7个以下,则环氧树脂之间的灵活的键合力稍微降低,若乙氧基在25个以上,则因链的长度过长而无法起到固化剂的作用。
优选地,上述化学式1的聚硫代化合物的重均分子量为660~1300。并且,优选地,在上述化学式1的聚硫代化合物中,相对于硫醇化合物的重量,-SH的含量为5~15重量%,-SH当量为220g/eq~450g/eq。
优选地,相对于100重量份的环氧树脂,包含100~200重量份的上述化学式1的聚硫代化合物。此时,在固化剂的含量少于100重量份的情况下,可能会使固化反应不充分,使耐热冲击性、降落冲击性及重操作性(修复性)等稍微变弱,而在固化剂的含量多于200重量份的情况下,可能因固化物中未反应的残留固化剂而使物性降低。
作为上述化学式2的巯基丙酸酯(Mercaptopropionate)硫醇化合物,可以使用三羟甲基丙烷三(3-巯基丙酸酯)(TMPMP,Trimethylol-propaneTri-3-Mercaptopropionate)、乙二醇二-3-巯基丙酸酯(GDMP,GlycolDi-3-Mercaptopropionate)、丙二醇-3-巯基丙酸酯(PPGMP,PropyleneGlycol-3-Mercaptopropionate)及季戊四醇四-3-巯基丙酸酯(PETMP,PentaerythritolTetra-3-Mercaptopropionate)等,但并不局限于此。
优选地,由本发明的化学式1表示的高分子量的聚硫代化合物包含在40~100重量份范围内,由化学式2表示的低分子量的聚硫代化合物包含在20~60重量份范围内。
在所混合的上述固化剂的含量少的情况下,可能会使固化反应不充分,使耐热冲击性、降落冲击性及重操作性(修复性)等稍微变弱,而在所混合的上述固化剂的含量多的情况下,可能因固化物中未反应的残留固化剂而使物性降低。本发明的环氧树脂组合物可以为上述环氧树脂和固化剂相互混合的单组分,或者上述环氧树脂和固化剂分开分离保管并在使用时相混合的双组分。环氧树脂组合物优选为单组分。
并且,除了上述环氧树脂及固化剂之外,本发明的环氧树脂组合物还可以包含固化促进剂。虽然这些三种成分全部优选为混合的单组分,但并不局限于此。上述固化促进剂只要是能够促进固化反应的,就可以任意使用,可以使用胺化合物、改性胺化合物、咪唑化合物及改性咪唑化合物等。作为上述胺化合物,可以利用双氰胺、二乙烯三胺、间苯二甲胺(m-Xylylenediamine)及异佛尔酮二胺等,作为改性胺化合物,可以利用在上述胺化合物附加环氧化合物的环氧附加聚胺等,作为咪唑化合物,可以利用2-甲基咪唑、2-乙基-4甲基咪唑及2-苯基咪唑等,作为改性咪唑化合物,可以利用在上述咪唑化合物附加环氧化合物的咪唑附加物等,但并不局限于此。优选地,固化促进剂的使用量以100重量份的环氧树脂为基准,包含0.1~10重量份。此时,在固化促进剂的含量少于0.1重量份的情况下,可能会因固化速度慢而使生产率下降,在固化促进剂的含量多于10重量份的情况下,可能会因保管时间及有用时间(availabletime)过短而使用不便。
另一方面,根据需要,本发明的耐冲击性优秀的环氧树脂组合物还可以包括脱泡剂、匀染剂、染料、颜料及填充剂等其他添加物。这些添加物可在能够实现本发明的目的的范围内少量包含。
另一方面,底部填充用密封剂以上述的本发明的环氧树脂组合物为主要成分来制备。并且,本发明的环氧树脂组合物虽然为了球栅陈列封装件或芯片尺寸封装件等半导体封装件的底部填充而创作的,但还可以在将半导体芯片搭载于载体基板上时使用。并且,由于其使用范围并不局限于底部填充用密封剂,因而在组装两种以上的部件的情况下,可以为了提高粘结性和密封性而使用。例如,还可以使用为液晶显示面板等的密封剂。并且,这种密封剂虽然以上述环氧树脂组合物为必需成分,但还可以包含选自增粘剂、相稳定剂及无机物填充剂等的一种以上的附加成分。
实施例1~实施例2及比较例1~比较例5
环氧树脂组合物的制备
如下列表1所示,以使环氧树脂、固化剂及固化促进剂的成分及含量不同的方式进行混合、脱泡,由此制备了环氧树脂组合物。
表1
环氧树脂组合物的成分及含量,单位:重量份
实验例1
(1)回路基板试片的制作(安装)
在配线基板的电极上印刷涂敷焊锡浆料,并在焊锡浆料上搭载芯片尺寸封装件之后,通过回流焊方法实施焊锡接合。此时,芯片尺寸封装件使用一边的长度为12mm的正四角形且端子数为176销的。之后,在芯片尺寸封装件的周围喷射、涂敷所制备的上述各实施例及比较例的环氧树脂组合物,使上述环氧树脂组合物向配线基板和芯片尺寸封装件之间渗透之后,在120℃条件下加热20分钟,从而使上述环氧树脂组合物固化。
如上所述,按不同组合物分别制作100个试片之后,对耐热冲击性、降落冲击性及重操作性进行评价,并将结果显示于下列表2中。
(2)耐热冲击性试验(温度循环性)
在低温侧-55℃、高温侧125℃条件下分别将维持时间定为30分钟的一小时为一循环,并在100循环下对试样进行导通试验,从而确认了配线基板和芯片尺寸封装件之间的电连接。此时,将在100循环内因断线等而非导通的试片判定为不良试片,并以(不良发生试片数)/(总试片数)来表示。
(3)降落冲击性试验
将试片从1.2m高度向混凝土上降落100次之后,进行导通试验,来确认了配线基板和芯片尺寸封装件之间的电连接。此时,在降落之后,将非导通的试片判定为不良试片,并以(不良发生试片数)/(总试片数)来表示。
(4)冲击弯曲性(碰撞弯曲性)
在配线基板中,将被环氧树脂组合物密封的芯片尺寸封装件置于离底面5cm左右之后,固定配线基板的四角部分,并在离芯片尺寸封装件边缘约1cm左右的高度使用末端呈圆的直径为2mm以下的棒,以每秒一次利用1kgf的力反复进行冲击试验。每隔10次使用显微镜观察环氧树脂的裂开程度,并标注该次数。
(5)重操作性试验(修复性)
在配线基板中,利用热风发生器对被环氧树脂组合物密封的芯片尺寸封装件的附近施加1分钟260℃左右的热风来加热。并且,在配线基板和芯片尺寸封装件之间插入刮刀,将芯片尺寸封装件抬起并剥离。之后,利用加热至300℃的焊锡烙铁去除了残留于配线基板上的树脂固化物和焊锡。并且,利用焊锡吸入用编织线去除残留于配线基板上的焊锡,并利用乙醇清洗了配线基板表面。然后,在以这种方式去除芯片尺寸封装件的配线基板上重新涂敷焊锡浆料,并重新安装了新的芯片尺寸封装件。之后,以与上述相同的方式将各实施例及比较例的环氧树脂组合物喷射、涂敷于芯片尺寸封装件周围,使上述环氧树脂组合物渗透之后,在120℃条件下加热20分钟,从而使环氧树脂组合物固化。对所修复的试片,以与上述的方法相同的方法进行耐热冲击试验和降落冲击试验,将非导通的试片判定为不良试片,并以(不良发生试片数)/(总试片数)来表示。
表2
评价结果
实施例1 | 实施例2 | 比较例1 | 比较例2 | 比较例3 | 比较例4 | 比较例5 | |
耐热冲击性 | 0/100 | 0/100 | 6/100 | 8/100 | 8/100 | 10/100 | 3/100 |
降落冲击性 | 0/100 | 0/100 | 3/100 | 0/100 | 30/100 | 15/100 | 100/100 |
冲击弯曲性 | 900 | 1000 | 400 | 500 | 200 | 300 | 5 |
重操作性 | 0/100 | 0/100 | 2/100 | 0/100 | 50/100 | 20/100 | 70/100 |
如上述表2所示,可以确认混合高分子量的巯基丙酸酯类化合物及低分子量的巯基丙酸酯类化合物的本发明的组合物(实施例1及实施例2)与单独的高分子量的巯基丙酸酯类化合物(比较例1及比较例2)、单独的低分子量的巯基丙酸酯类化合物(比较例3及比较例4)相比,在耐热冲击性、降落冲击性、冲击弯曲性及重操作性方面显著优秀。
上述实施例仅为本发明的实施例,本发明并不局限于上述实施例,本发明可在发明要求保护范围所记载的范围内实施多种变形是显而易见的。
产业上的可利用性
本发明涉及用作半导体封装件等电子材料密封剂的环氧树脂组合物,更详细地,涉及包含高分子量的聚硫代化合物作为环氧树脂的固化剂的环氧树脂组合物。
Claims (4)
1.一种热固性环氧树脂组合物,包含分子内具有两个以上的环氧基的环氧树脂、环氧树脂固化剂及固化促进剂,上述热固性环氧树脂组合物的特征在于,
相对于100重量份的环氧树脂,上述环氧树脂固化剂包含:
a)40~100重量份的由以下化学式1表示的高分子量的聚硫代化合物,
b)20~60重量份的由以下化学式2表示的低分子量的聚硫代化合物;
化学式1:
在上述化学式中,
R为氢、甲基或乙基,
x、y、z为0或整数,x、y、z之和为7~25;
化学式2:
在上述化学式中,R为氢、甲基或乙基,m为0~2,n为2~4整数,m、n之和为4。
2.根据权利要求1所述的热固性环氧树脂组合物,其特征在于,上述化学式1的聚硫代化合物的重均分子量为660~1300。
3.根据权利要求1所述的热固性环氧树脂组合物,其特征在于,相对于聚硫代化合物的重量,上述化学式1的聚硫代化合物的-SH含量为5~15重量%,-SH当量为220g/eq~450g/eq。
4.根据权利要求1至3中任一项所述的热固性环氧树脂组合物,其特征在于,上述固化促进剂为胺化合物、咪唑化合物。
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