CN102209804A - 磊晶成长膜形成用高分子积层基板及其制造方法 - Google Patents

磊晶成长膜形成用高分子积层基板及其制造方法 Download PDF

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CN102209804A
CN102209804A CN2009801443447A CN200980144344A CN102209804A CN 102209804 A CN102209804 A CN 102209804A CN 2009801443447 A CN2009801443447 A CN 2009801443447A CN 200980144344 A CN200980144344 A CN 200980144344A CN 102209804 A CN102209804 A CN 102209804A
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laminated substrate
polymer laminated
tinsel
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冈山浩直
南部光司
金子彰
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Toyo Kohan Co Ltd
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Abstract

本发明提供一种具有经高度结晶配向的表面的磊晶成长膜形成用高分子积层基板及其制造方法。所述制造方法包括：将高分子板T1的至少一个表面活化的步骤；将以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔T2的至少一个表面活化的步骤；使高分子板的活化表面与金属箔的活化表面相对向而积层并冷延的步骤；通过热处理使金属箔双轴结晶配向的步骤。

Description

磊晶成长膜形成用高分子积层基板及其制造方法
技术领域
本发明涉及一种用以形成磊晶成长膜的高分子积层基板及其制造方法。
背景技术
以前磊晶成长膜形成用基板是使用结晶配向性优异的单晶硅(Si)、单晶砷化镓(GaAs)、单晶蓝宝石(Al2O3)等单晶晶圆。
但是，这些单晶晶圆是尺寸即便较大也为300mmΦ左右的砧板，无法通过象卷到卷方式的连续的生产方式进行成膜。
另外，Si等也无强度，在制造步骤的搬送中，不容易操作而需要注意。
另外，所述单晶晶圆由于无法对基板赋予柔性，而所使用的用途也受到限定。
在所述单晶晶圆以外，使磊晶成长膜形成的基板已知：将Ni、Cu、Ag、或这些金属的合金以高压下率进行冷延，对材料整体赋予均匀的应变后，通过热处理使其再结晶，而形成高度双轴结晶配向性的金属基板。
其中，如专利文献1-专利文献5所示，提出Ni或Ni-W合金与其他金属材料的包层材料，但这些材料是中间层或超电导体层的成膜在大于等于600℃的高温下进行或降低饱和磁化、且使表面沿着(200)面结晶配向的材料，通常得不到普及，是特殊且高价的材料。
专利文献1：日本专利第3601830号公报
专利文献2：日本专利第3587956号公报
专利文献3：WO2004/088677号公报
专利文献4：日本专利特开2006-286212号公报
专利文献5：日本专利特开2007-200831号公报
如所述说明，磊晶成长膜的形成用单晶晶圆基板可以列举以下问题。
即，使用高价的单晶基板；单晶基板尺寸也较小，必须进行单片式的步骤处理；基板坚硬、无法赋予柔性；应用面受到限定。
发明内容
因此，本发明的目的是为了解决所述问题而提出具有高度结晶配向的表面的磊晶成长膜形成用高分子积层基板及其制造方法。
(1)本发明的磊晶成长膜形成用高分子积层基板的制造方法的特征在于：在高分子板上积层以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔，积层后通过热处理使所述金属箔进行双轴结晶配向。
(2)本发明的磊晶成长膜形成用高分子积层基板的制造方法的特征在于：包括将高分子板的至少一个表面活化的步骤；将以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔的至少一个表面活化的步骤；使所述高分子板的活化表面与所述金属箔的活化表面相对向而积层并冷延的步骤；通过热处理使所述金属箔进行双轴结晶配向的步骤。
(3)本发明的磊晶成长膜形成用高分子积层基板的制造方法的特征在于：包括通过溅镀在高分子板的至少一个表面形成金属层的步骤；将以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔的至少一个表面活化的步骤；使所述高分子板的金属层表面与所述金属箔的活化表面相对向而积层并冷延的步骤；通过热处理使所述金属箔进行双轴结晶配向的步骤。
(4)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据(2)或(3)所述，其特征在于：所述积层时的冷延的压下率小于等于10％。
(5)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据所述(1)至(4)中任一项所述，其特征在于：进行将所述金属箔侧表面的表面粗度Ra调整为大于等于1nm且小于等于40nm的双轴结晶配向。
(6)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据所述(1)至(5)中任一项所述，其特征在于：所述金属箔的厚度为大于等于7μm且小于等于50μm。
(7)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据所述(1)至(6)中任一项所述，其特征在于：所述热处理温度为大于等于150℃且小于等于400℃。
(8)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据所述(1)至(7)中任一项所述，其特征在于：所述金属箔包含总计大于等于0.01％且小于等于1％的Ag、Sn、Zn、Zr、O、N。
(9)本发明的磊晶成长膜形成用高分子积层基板的制造方法根据所述(1)至(8)中任一项所述，其特征在于：在通过所述高分子积层基板的制造方法而制造的高分子积层基板的金属面上，进一步形成保护膜。
(10)本发明的磊晶成长膜形成用高分子积层基板的特征在于：其是通过根据所述(1)至(9)中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法而制造。
发明的效果
本发明的磊晶成长膜形成用高分子积层基板由于以高分子为基板，因此具有柔性，由于具有经高度结晶配向的表面，因此作为磊晶成长膜形成用基板而较为优异。
附图说明
图1为本发明的实施方式的高分子积层基板5A的构成的概略截面图。
图2为本发明的实施方式的高分子积层基板5B的构成的概略截面图。
图3为本发明的实施方式的高分子积层基板10A的构成的概略截面图。
图4为本发明的实施方式的高分子积层基板10B的构成的概略截面图。
图5为表面活化接合装置D1的概略图。
【主要组件符号说明】
Figure BPA00001363028000031
具体实施方式
图1是表示本发明的磊晶成长膜形成用高分子积层基板5A的构成的概略截面图。
如图1所示，高分子积层基板5A具备：高分子板T1、积层在高分子板T1上的金属箔T2。
高分子板T1根据其使用目的而进行选择，如果可以承受所贴合的金属箔T2的再结晶热处理温度150℃-400℃，则可以应用，其中由于耐热性优异，并且通常普及的聚酰亚胺、液晶聚合物、芳香族聚酰胺等树脂膜的高温耐热性优异，因而可优选列举。
高分子板T1的厚度如果能确保强度，并且能以宽幅、长条线圈的状态提供，则并无特别限定，如果考虑到成本面或普及的芳香族聚酰胺膜、聚酰亚胺膜或液晶聚合物膜，则较理想的是大于等于3μm且小于等于200μm。
金属箔T2可以列举Cu箔或Cu合金箔(本说明书中将两者合并称为Cu合金箔)作为优选的材料。
Cu合金箔T2以事先通过热处理而结晶配向的状态使用，操作过程中有产生应变，使结晶配向性劣化的危险性，因此较理想的是Cu合金箔T2与高分子板T1积层而形成高分子积层基板后赋予高度的结晶配向性。
因此，本发明的Cu合金箔T2在与高分子板T1积层前，优选为通过压下率大于等于90％的强加工而形成的均匀的压延集合组织的状态。
原因是如果压下率小于90％，则之后进行的热处理中有可能Cu不会发生配向。
这种高压下压延Cu合金箔是为了在柔性安装基板用途中赋予高弯曲性而开发并普及，而可以容易获得。
例如可以列举：日矿材料(Nikko-Materials)公司制造的高压下压延Cu箔(HA箔(商品名))或日立电线公司制造的高压下压延Cu箔(HX箔(商品名))等。
本发明中，如上所述的市售品的高压下压延Cu合金箔由于结晶配向性优异，而使用较理想。
较理想的是厚度大于等于7μm且小于等于50μm。更优选为12μm-18μm。将厚度设定大于等于7μm的理由是为了确保Cu合金箔T2的强度，将厚度设定小于等于50μm的理由是为了确保Cu合金箔T2的加工性。
至于Cu合金箔T2的结晶配向，是在Cu合金箔T2与高分子板T1接合时或接合后的目标磊晶成长膜形成步骤中，通过将高分子积层基板的温度设定为大于等于150℃，而在接合时或目标磊晶成长膜形成步骤中使Cu合金箔再结晶化，从而赋予高度的结晶配向性。
但是，在接合时或接合后的目标磊晶成长膜形成步骤中，在高分子积层基板的温度低于150℃的低温下进行处理时，或者即便在大于等于150℃通过步骤而连续步骤的处理时间也较短时，Cu合金箔的再结晶化会受到抑制，而无法赋予高度的结晶配向性，因此优选事先通过热处理而事先使高分子积层基板上的Cu合金箔结晶配向。
热处理温度是大于等于Cu合金箔的再结晶结束的温度即可，如果考虑到接合对象是高分子板，其耐热性或使结晶配向性为大于等于99％的高配向率等，则较理想的是热处理温度为大于等于150℃且小于等于400℃。
所述Cu合金箔中如果有能通过热处理容易以(200)面结晶配向率大于等于99％进行配向的元素，则可为任意添加元素，可以添加微量Ag、Sn、Zn、Zr、O、N，但总计含量大于等于0.01％且小于等于1％。
将添加元素总计设定为小于等于1％的理由是虽然添加元素与Cu会形成固溶体，但如果添加元素总计超过1％，则会导致固溶体以外的氧化物等杂质增加，而有可能影响配向。
因此，优选总计为大于等于0.01％且小于等于0.1％。
通过将所述说明的高分子板与Cu合金箔接合，而完成高分子积层基板。
另外，图2表示在高分子板T1的两面接合金属箔T2的实施方式的高分子积层基板5B。
图2的高分子积层基板5B由于在柔性高分子板T1的两面积层有结晶配向金属层，因此可制成使磊晶成长膜在两面成长的基板。
高分子板与Cu合金箔的接合方法只要可将宽幅且长条线圈沿着长度方向均匀接合，则可为任意方法，可以列举：使用粘结剂通过双辊进行压接的方法；或不使用粘结剂而直接将高分子板与Cu合金箔接合的浇铸方式等。
另外，也较理想的是使用在接合后也能获得稳定结晶配向性的表面活化接合法。
表面活化接合法例如可以列举图5所示的真空表面活化接合装置D1。所谓表面活化接合，是指通过溅镀蚀刻等方法将表面的氧化物或污垢等去除，而使所积层的高分子板或金属箔的表面活化，并使经活化的表面与其他积层物抵接而进行冷延。另外，可以在高分子板的表面通过溅镀设置金属层。
如图5所示，以宽度150mm～600mm的长条线圈的形态准备高分子板24及Cu合金箔26，分别设置于表面活化接合装置D1的卷取部62、64。
从卷取部62、64搬送的高分子板24及Cu合金箔26被连续地搬送到表面活化处理步骤，因此事先将所接合的2个面活化处理后进行冷压接。
表面活化处理步骤中，在10Pa～1×10-2Pa的极低压惰性气体环境中，将具有接合面的高分子板24与Cu金属箔26分别设为地线接地的一电极A(72、82)，在电极A(72、82)与经绝缘支持的另一电极B(74、76及84、86)之间施加1MHz～50MHz的交流电而产生辉光放电，且以通过辉光放电而产生的等离子体中所露出的电极的面积小于等于电极B面积的1/3的方式进行溅镀蚀刻处理。
惰性气体可以使用：氩气、氖气、氙气、氪气等、或包含至少一种这些气体的混合气体。
在溅镀蚀刻处理中，利用惰性气体将高分子板24及Cu金属箔26接合的面进行溅镀，从而去除表面吸附层及表面氧化膜，而使接合的面活化。该溅镀蚀刻处理中，电极A(72、82)采用冷却辊的形态，防止各搬送材料的温度上升。
然后，连续地搬送到压接辊步骤，将经活化的面彼此压接。压接下的环境气体如果存在O2气体等，则搬送中经活化处理的面会再次被氧化，而对密接造成影响。因此，较理想的是在小于等于1×10-3Pa的高真空下进行。另外，压下率越低则厚度精度越优异，且不会破坏金属箔的状态，因此压下率优选小于等于10％。压下率更优选小于等于2％。
通过所述压接步骤而密接的积层体被搬送到卷绕步骤，于此进行卷绕。
另外为了提高高分子板与Cu合金箔的密接性，也较为有效的是，利用电极B(74)对高分子板进行溅镀蚀刻后，设置Ni、Ni-Cr合金或Ni-Cu合金等靶，而在高分子板的接合面侧形成金属中间层。
另外，如图3所示，在Cu合金箔上形成目标膜而且无法确保密接性时，或难以直接在Cu上进行磊晶成长时，可在高分子积层基板上形成保护膜作为中间层。
例如，在蓝色发光二极管用途中，以半导体化合物的形式形成GaN膜来作为磊晶成长膜时，可在Cu合金箔上形成InGaN层或ZnO层作为保护膜，再于保护膜上形成GaN膜。
至于保护膜的厚度，为了发挥出防止底层的Cu的扩散的功能，为大于等于0.1μm即可。另外，为了维持磊晶成长膜，保护膜的厚度优选小于等于10μm。
保护膜的形成方法一般认为有溅镀法、蒸镀法、CVD(Chemical Vapor Deposition，化学气相沉积)法、MOCVD(Metal-Organic Chemical Vapor Deposition，有机金属化学气相沉积)法、电解镀敷法、无电解镀敷法等，可以是任一种方法。将保护膜设为Ni等金属时，于经济方面而言优选电解镀敷法。另外，将氧化物或氮化物作为保护膜时，优选在基板温度相对较低的低温下能成膜的溅镀法或MOCVD法等。
另外，图4表示在高分子板T1的两面接合金属箔T2，并在各金属箔T2上形成保护膜T3的实施方式的高分子积层基板10B。
图4的高分子积层基板10B由于在柔性高分子板T1的两面积层结晶配向金属层，并且在各金属箔T2上形成保护膜T3，因此可制成使磊晶成长膜在两面成长的基板。
另外，磊晶成长膜的形成方法可以使用：电解镀敷法、无电解镀敷法、真空蒸镀法、溅镀成膜法等公知的方法。
磊晶成长膜的膜厚必须达到磊晶成长的膜，较理想的是大于等于1nm且小于等于10μm。
原因是，在磊晶成长膜的膜厚小于1nm时，无法确保所形成的膜的密接性，在磊晶成长膜的膜厚超过10μm时，膜厚会过厚。
接着，对高分子积层基板上的经结晶配向的Cu合金箔的表面粗度进行说明。
Cu合金箔的表面粗度在购入时，如果表面粗度Ra为小于等于40nm，则无问题，也有表面粗度Ra超过100nm的Cu合金箔。
合金箔的表面粗度(称为平均表面粗度)Ra为100nm时也具有作为基板的充分的性能，但是表面粗度Ra越低，则结晶配向性越好，因此在Ra为100nm的表面粗度状态时，在表面活化接合后，进行将表面粗度Ra调整为小于等于40nm的处理。
使表面粗度降低的方法认为有：利用压延辊的压下、抛光研磨、电解研磨或电解研磨粒研磨等，可以为任一种方法。表面粗度较理想的是镜面，考虑到目前的方法及经济性，较理想的是将Ra设定为大于等于1nm且小于等于10nm。
通过调整为象所述一样的表面粗度，而可以形成更优异的磊晶成长膜用高分子积层基板，并在这样的基板上形成高性能的功能性膜。
通过以所述方式制造磊晶成长膜用高分子板，而可以一直保持Cu金属箔的以高压下率进行冷延的状态并以界面平滑的状态积层在高分子板上。然后进行加热使金属箔双轴结晶配向时，如果未保持Cu金属箔的以高压下率进行冷延的状态，则表现不出必需的双轴结晶配向。另外，如果界面不平滑则会导致双轴结晶配向破坏。
而且，在使用表面活化接合进行积层时，即便通过积层后的加热，产生变形等的可能性也较少，因此导致双轴结晶配向破坏的可能性也较少，与使用粘结剂等的情况相比，更加有利。
实施例1
以下，揭示本发明的实施例，对所得的高分子积层基板的特性进行说明。
分别将200mm宽的18μm厚的高压下压延Cu箔与100μm厚的聚酰亚胺膜以及液晶聚合物膜，通过常温表面活化接合法接合后，在200℃下进行5分钟热处理而获得高分子积层基板。
表1表示此时的Cu(200)面与Cu箔表面平行的比例、即结晶配向率(通过X射线衍射而测定的θ/2θ衍射波峰的(200)面的衍射波峰强度率：I(200)/∑I(hkl)×100(％))，及作为表示此(200)面与长度方向<001>平行的值的双轴配向性指标的ΔΦ°(X射线衍射所得Ni(111)极点图中获得的Φ扫描波峰(α＝35°的4条波峰的半值宽度的平均值))。
比较例是表示在130℃下进行热处理时，以及将非一般的高压下的16μm厚的压延Cu箔通过所述常温活化接合法接合后，在200℃下进行5分钟热处理时的波峰强度。
根据表1可知，高压下压延Cu箔与所积层的高分子板的种类无关，在热处理温度为130℃×5分钟时，结晶配向率为93％，仍然说不上充分，在200℃下保持5分钟，则(200)面结晶配向率大于等于99％。
另外，比较例所示的使用通常的压延Cu箔时，即便进行热处理结晶配向率也小于等于70％。
另外，结晶配向率大于等于99％的实施例的ΔΦ为6°，表现出相当高的双轴结晶配向度。
[表1]
Figure BPA00001363028000091
另外，所述测定值是在200mm的宽度方向上测定板的两端附近与中央的计3处的平均值，宽度方向上的值几乎未见到差异。
在Cu箔表面保持均匀的结晶配向性的状态下，将本发明的高分子积层基板制造为宽幅且长条线圈，因此可以期待用作各种磊晶成长膜用基板。
磊晶成长膜的形成方法有镀敷法、物理蒸镀(PVD，physical vapor deposition)法、化学蒸镀(CVD，chemical vapor deposition)法、分子束(MBE，molecular beam epitaxy)法等。
所述磊晶成长膜的形成方法在逐年地发展，例如CVD法中代替至今为止将成膜基板温度提高到400～800℃而进行的方法，而开发出通过使用RF离子体而能在基板温度为200℃左右下成膜的方法，可实现多晶Si膜或GaN等的低温成膜。
本发明的高分子积层基板通过所述低温成膜的技术，而可以用作太阳电池用多晶硅(Si)膜、发光二极管用氮化镓(GaN)膜、可以期待催化剂-光电效果等的TiO2膜等各种磊晶成长膜用基板。
产业上的可利用性
本发明的磊晶成长膜形成用高分子积层基板的制造方法可以通过使用长条线圈而进行卷到卷方式的连续成膜步骤。
而且，能有助于太阳电池用多晶硅膜的结晶配向化、轻量化或柔性的赋予、发光二极管用GaN元件的低价格化等，可以用作至今为止仍未研究的领域中的磊晶成长膜用新材料，在产业上极为有用。

Claims (10)

1.一种磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：在高分子板上积层以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔，积层后通过热处理使所述金属箔进行双轴结晶配向。
2.一种磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：包括将高分子板的至少一个表面活化的步骤；
将以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔的至少一个表面活化的步骤；
使所述高分子板的活化表面与所述金属箔的活化表面相对向而积层并冷延的步骤；
通过热处理使所述金属箔双轴结晶配向的步骤。
3.一种磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：包括通过溅镀在高分子板的至少一个表面形成金属层的步骤；
将以压下率大于等于90％进行冷延的包含Cu或Cu合金的金属箔的至少一个表面活化的步骤；
使所述高分子板的金属层表面与所述金属箔的活化表面相对向而积层并冷延的步骤；
通过热处理使所述金属箔双轴结晶配向的步骤。
4.根据权利要求2或3所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：所述积层时的冷延的压下率小于等于10％。
5.根据权利要求1至4中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：进行将所述金属箔侧表面的表面粗度Ra调整为大于等于1nm且小于等于40nm的双轴结晶配向。
6.根据权利要求1至5中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：所述金属箔的厚度为大于等于7μm且小于等于50μm。
7.根据权利要求1至6中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：所述热处理温度为大于等于150℃且小于等于400℃。
8.根据权利要求1至7中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：所述金属箔总计包含大于等于0.01％且小于等于1％的Ag、Sn、Zn、Zr、O、N。
9.根据权利要求1至8中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法，其特征在于：在通过所述高分子积层基板的制造方法而制造的高分子积层基板的金属面上，进一步形成保护膜。
10.一种磊晶成长膜形成用高分子积层基板，其特征在于：其是通过根据权利要求1至9中任一项所述的磊晶成长膜形成用高分子积层基板的制造方法而制造。
CN2009801443447A 2008-11-12 2009-10-20 磊晶成长膜形成用高分子积层基板及其制造方法 Pending CN102209804A (zh)

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