CN116224716A - 一种用于hjt太阳能电池铜栅制备的光刻胶及其制备方法 - Google Patents
一种用于hjt太阳能电池铜栅制备的光刻胶及其制备方法 Download PDFInfo
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- CN116224716A CN116224716A CN202310336834.9A CN202310336834A CN116224716A CN 116224716 A CN116224716 A CN 116224716A CN 202310336834 A CN202310336834 A CN 202310336834A CN 116224716 A CN116224716 A CN 116224716A
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Abstract
本发明公开了一种用于HJT太阳能电池铜栅制备的光刻胶及其制备方法,所述光刻胶包含按重量份数计的以下组分:粘结剂聚合物30‑60份、光反应性单体10‑45份、光引发剂1‑5份;所述粘结剂聚合物由丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯和甲基丙烯酸环氧丙酯在光引发剂以及溶剂存在下自由基聚合得到,所述丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯、甲基丙烯酸环氧丙酯的摩尔比为1:1‑1.2:0.8‑1.1:0.9‑1.1:1‑1.2,所述粘结剂聚合物的分子量大于6000。本发明制备的一种光刻胶具有快速固化、快速显影、易去胶的特点,同时具有高解析度和优异的显影性,可用于铜栅异质结电池的制备。
Description
技术领域
本发明涉及异质结电池技术领域,具体涉及一种用于HJT太阳能电池铜栅制备的光刻胶及其制备方法。
背景技术
银浆是异质结(HJT)光伏电池的关键原材料,是由高纯度(99%)的银粉、玻璃氧化物、有机材料等所组成的机械混合物的粘稠状浆料,应用在HJT电池生产的最后一步主工艺环节-金属化,通过在电池两侧印刷固化金属电极,使得电极与电池片紧密结合,形成高效的欧姆接触以起到导电作用,直接影响光伏电池的光电转换效率。HJT电池银浆消耗量大,降本突破点在于银浆。
使用其它金属替代部分银粉,例如银包铜、电镀铜,是降本的有效途径。相比较而言,铜电镀的成本优势明显,传统丝网印刷的金属化成本约为0.2元/瓦,铜电镀的成本约为0.1元/瓦。由于铜电镀通过在底部生长的方式,只要有电子交换,铜离子就会在电子产生的地方沉积,所以铜电镀栅线的宽度更小,可以使得电池片放置更多的栅线,从而能有效提高电池片发电效率。但目前铜栅的制备通常采用干膜,干膜经压膜、曝光、撕膜、显影、电镀形成电极栅极,干膜的成本高,且制备的栅线精度低。因此,亟需一种快速固化、快速显影且易去胶的高感度光刻胶,可有效提高栅线的制备精度,从而提升异质结太阳能电池的生产效率及良率。
发明内容
本发明要解决的技术问题是提供一种用于HJT太阳能电池铜栅制备的光刻胶及其制备方法,该光刻胶具有快速固化、快速显影、易去胶,可有效提高铜栅线的制备精度以及制备效率。
为了解决上述技术问题,本发明提供以下技术方案:
本发明第一方面提供了一种用于HJT太阳能电池铜栅制备的光刻胶,所述光刻胶包含按重量份数计的以下组分:粘结剂聚合物30-60份、光反应性单体10-45份、光引发剂1-5份;
所述粘结剂聚合物由丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯和甲基丙烯酸环氧丙酯在引发剂以及溶剂存在下通过自由基聚合得到,所述丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯、甲基丙烯酸环氧丙酯的摩尔比为1:1-1.2:0.8-1.1:0.9-1.1:1-1.2;
所述粘结剂聚合物的重均分子量大于6000。
本发明采用大量含羧基的单体用于制备粘结剂聚合物,有利于成膜后的光刻胶易与在后续的碱性显影液中溶解去胶。同时,引入异戊二烯以及带甲基的丙烯酸单体,可改善树脂的成膜性能,防止镀铜过程中膜层开裂导致渗镀的现象;另外,引入的含氟单体以及含环氧基团的单体可有效提高聚合物的稳定性以及亲水性能。
进一步地,所述丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯、甲基丙烯酸环氧丙酯的摩尔比更优选为1:1.1:1:1:1.1。
进一步地,所述引发剂优选为偶氮二异丁腈;以摩尔量计,所述引发剂的加入量为制备粘结剂聚合物单体总量的0.05%-0.5%,例如0.1%、0.2%、0.3%、0.4%等。
进一步地,所述溶剂为丙二醇甲醚醋酸酯;以质量计,所述丙二醇甲醚醋酸酯的加入量占总反应物质量的50%-80%,总反应物包括制备粘结剂聚合物单体、引发剂以及丙二醇甲醚醋酸酯。
进一步地,所述自由基聚合的反应温度为70-90,反应时间为6-10h。
进一步地,所述粘结剂聚合物的重均分子量为6000-9000,分子量分布为1.3-1.7。本发明制备的光刻胶中包含的粘结剂聚合物分子量不可过高,采用超高分子量粘结剂聚合物制备的光刻胶的粘度会比较大,从而不利于后期的碱洗去胶;但粘结剂聚合物分子量也不可过低,采用分子量过低的粘结剂聚合物制备的光刻胶在成膜过程中易发生开裂现象。因此,本发明用于制备光刻胶的粘结剂聚合物的分子量需适中,例如重均分子量为6000-9000的粘结剂聚合物,可保证成膜性的同时易于去胶。
进一步地,所述光反应性单体为丙烯酸酯类单体,具有如下结构通式:
其中,所述R1为氢或甲基;
所述R2为C1-C12的烷基、取代或为取代的苯基,所述取代的苯基中取代基为C1-C4的烷基、C1-C4的烷氧基、卤素、氰基、羧酸、酯基、环烷基或胺基,更优选为C1-C8的烷基或C1-C8的烷氧基酯。
进一步地,所述光反应性单体可选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸-2-羟基甲酯、丙烯酸-2-羟基乙酯、丙烯酸-2-羟基丙酯、丙烯酸-2-羟基丁酯中的一种或多种。
进一步地,所述光引发剂选自苯偶姻类、安息香醚类、二苯甲酮类、米氏酮类、苯乙酮类、吖啶类、蒽醌类、缩酮类、有机卤化物类、重氮萘醌类、有机过氧化物类、硫醇类、噻唑酮类、苯基膦氧类、六芳基咪唑类、香豆素类、噁唑类、吡唑啉类或三芳基胺类化合物中的一种或多种。
进一步地,所述光引发剂可选自苯偶姻、苯偶姻甲基醚、苯偶姻乙基醚、苯偶姻异丙基醚、苯偶姻苯基醚、二苯甲酮、4,4’-双(二甲胺基)二苯甲酮、4,4’-双(二乙胺基)二苯甲酮、4-甲氧基-4’-二甲胺基二苯甲酮、2-苄基-2-二甲胺基-1-(4-吗啉基苯基)-丁酮-1、2-甲基-1-[4-(甲基硫基)苯基]-2-吗啉基-丙酮-1、苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2,2-二乙氧基-2-苯基苯乙酮、1,1-二氯苯乙酮、9-苯基吖啶,9-烷基吖啶、2-甲基蒽醌、2-乙基蒽醌、2-叔丁基蒽醌、1-氯蔥醌、9,10-二甲氧基蒽、9,10-二乙氧基蒽、9,10-二丙氧基蒽、9,10-二丁氧基蒽、苄基二甲基缩酮、三溴甲基苯砜、重氮萘醌磺酸酯、过氧化苯甲酰、过氧化异丙苯、2-巯基苯并咪唑、2-巯基苯并噁唑、2-巯基苯并噻唑、2,4-二甲基噻唑酮、2,4-二乙基噻唑酮、2-氯噻唑酮、2,4-二异丙基噻唑酮、过氧化苯甲酰、2-(邻氯苯基)-4,5-二苯基咪唑二聚物、2-(邻氯苯基)-4,5-二(甲氧基苯基)咪唑二聚物中的一种或多种。
进一步地,所述光刻胶还包含交联剂、流平剂、表面活性剂、阻聚剂、稳定剂、分散剂、增塑剂、染色剂中的一种或多种。
进一步地,所述交联剂优选为二甲基丙烯酸乙二醇酯和/或双三羟甲基丙烷三丙烯酸酯。
进一步地,所述流平剂优选为迪高,更优选迪高4100。
进一步地,所述表面活性剂优选为含氟表面活性剂或硅氧烷表面活性剂。
进一步地,所述阻聚剂优选为苯二酚、对羟基苯甲醚、2,6-二叔丁基对甲苯酚、2,5-二叔丁基对苯二酚、2-叔丁基对苯二酚、对苯醌中的一种或多种。
进一步地,所述稳定剂优选为举磷酸、亚磷酸、草酸、苯磺酸中的一种或多种。
进一步地,所述分散剂优选为油酸钠和/或季胺盐。
进一步地,所述增塑剂优选为磷酸三丁酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯中的一种或多种。
进一步地,所述染色剂优选为结晶紫、维多利亚蓝、酞菁绿中的一种或多种。
进一步地,所述光刻胶还包含溶剂,所述溶剂甲醇、乙醇、丙醇、丁醇、丙酮、丁酮、N-甲基2-吡咯烷酮、甲基乙基酮、乙二醇单甲醚、乙二醇单乙醚、乙二醇单丙醚、乙二醇单丁醚、甲苯、N,N’-二甲基甲酰胺、丙二醇单甲醚、二甲基亚砜、二乙基亚砜、苯酚、邻甲酚、间甲酚、对甲酚、二甲苯酚、卤代苯酚、邻苯二酚、四氢呋喃、二恶烷、二氧戊环、环丙二醇甲醚、四乙二醇二甲醚、γ-丁内酯、六甲基邻酰胺、丙二醇甲醚醋酸酯中的一种或多种。
进一步地,所述光刻胶更优选包含按重量份数计的以下组分:粘结剂聚合物30-40份、光反应性单体15-30份、光引发剂2-4份,交联剂1~3份、流平剂0.5~1.5份以及溶剂100~150份。
本发明第二方面提供了第一方面所述光刻胶的制备方法,将光刻胶中各组分根据配方量混合均匀,过滤后得到所述光刻胶。
与现有技术相比,本发明的有益效果:
本发明提供了一种用于HJT太阳能电池铜栅制备的光刻胶,该光刻胶易于涂布,可快速热固化、显影,光刻胶的形貌陡直度可达到80°以上,电镀后胶面无开裂或渗渡的现象,并且在电镀铜后,由光刻胶形成的膜可通过浸泡的方式去除,且去除后电池表面无胶残留,可有效提高异质结太阳能电池表面铜栅线的制备精度以及制备效率。
具体实施方式
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。本文所使用的术语“及/或”包括一个或多个相关的所列项目的任意的和所有的组合。
下面结合具体实施例对本发明作进一步说明,以使本领域的技术人员可以更好地理解本发明并能予以实施,但所举实施例不作为对本发明的限定。
实施例1
本实施例提供了一种用于铜栅异质结电池的高感度太阳能光刻胶,具体的制备方法如下:
(1)粘结剂聚合物的制备:将丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯和甲基丙烯酸环氧丙酯按摩尔比为1:1.1:1:1:1.1加至反应釜中,向反应釜中加入丙二醇甲醚醋酸酯,然后加入将溶有偶氮二异丁腈(AIBN)的丙二醇甲醚醋酸酯滴至反应釜中,在80℃条件下搅拌反应8h,得到粘结剂聚合物,测得重均分子量为7200;以摩尔量计,AIBN的用量为制备粘结剂聚合物单体的0.1%;丙二醇甲醚醋酸酯加入的量为反应釜中总物质量的65wt%;
(2)将165g步骤(1)制备的粘结剂聚合物与57g丙烯酸甲酯、48g丙烯酸-2-羟基甲酯、10g光引发剂二苯甲酮、5g光引发剂2,2-二甲氧基-2-苯基苯乙酮、9g交联剂二甲基丙烯酸乙二醇酯、6g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
实施例2
本实施例提供了一种用于铜栅异质结电池的高感度太阳能光刻胶,具体的制备方法如下:
(1)粘结剂聚合物的制备:与实施例1相同;
(2)将171g步骤(1)制备的粘结剂聚合物与54g丙烯酸甲酯、45g丙烯酸-2-羟基甲酯、8.5g光引发剂二苯甲酮、5g光引发剂2,2-二甲氧基-2-苯基苯乙酮、10.5g交联剂二甲基丙烯酸乙二醇酯、6g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
实施例3
本实施例提供了一种用于铜栅异质结电池的高感度太阳能光刻胶,具体的制备方法如下:
(1)粘结剂聚合物的制备:与实施例1相同;
(2)将159g步骤(1)制备的粘结剂聚合物、60g丙烯酸甲酯、51g丙烯酸-2-羟基甲酯、8g光引发剂二苯甲酮、7g光引发剂2,2-二甲氧基-2-苯基苯乙酮、10.5g交联剂二甲基丙烯酸乙二醇酯、4.5g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
对比例1
本对比例提供了一种光刻胶,具体的制备方法如下:
将165g市售改性丙烯酸树脂(ETERCURE 6071,分子量7000)、57g丙烯酸甲酯、48g丙烯酸-2-羟基甲酯、10g光引发剂二苯甲酮、5g光引发剂2,2-二甲氧基-2-苯基苯乙酮、9g交联剂二甲基丙烯酸乙二醇酯、6g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
对比例2
本对比例提供了一种光刻胶,具体的制备方法如下:
将171g市售改性丙烯酸树脂(长兴化工ETERCURE 6071,分子量7000)、54g丙烯酸甲酯、45g丙烯酸-2-羟基甲酯、8.5g光引发剂二苯甲酮、5g光引发剂2,2-二甲氧基-2-苯基苯乙酮、10.5g交联剂二甲基丙烯酸乙二醇酯、6g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
对比例3
本对比例提供了一种光刻胶,具体的制备方法如下:
(1)粘结剂聚合物的制备:将丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯和甲基丙烯酸环氧丙酯按摩尔比为1:1.1:1:1:1.1加至反应釜中,向反应釜中加入丙二醇甲醚醋酸酯,然后加入将溶有偶氮二异丁腈(AIBN)的丙二醇甲醚醋酸酯滴至反应釜中,在70℃条件下搅拌反应12h,得到粘结剂聚合物,测得数均分子量为5500;以摩尔量计,AIBN的用量为制备粘结剂聚合物单体的0.1%;丙二醇甲醚醋酸酯加入的量为反应釜中总物质量的65wt%;
(2)将165g步骤(1)制备的粘结剂聚合物与57g丙烯酸甲酯、48g丙烯酸-2-羟基甲酯、10g光引发剂二苯甲酮、5g光引发剂2,2-二甲氧基-2-苯基苯乙酮、9g交联剂二甲基丙烯酸乙二醇酯、6g流平剂迪高4100、400g溶剂丙二醇甲醚醋酸酯、200g溶剂乙二醇二乙醚混合搅拌均匀,再用0.5μm过滤器过滤,即得到相对应的光刻胶。
上述实施例及对比例制备的光刻胶的配方如下表1所示:
表1
应用及性能测试
将上述实施例及对比例制备的光刻胶用于电镀铜,具体操作如下:
利用旋转涂布机将光刻胶在太阳能电池片上涂覆,置于120℃的热板上烘烤5分钟,得到厚度为10~12μm的光刻胶层,然后用曝光机进行曝光,在置于2.38%的TMAH(晶瑞电材)中显影,然后用纯水冲洗,氮气吹干后进行电镀铜,电镀铜后去胶(电镀完成后用2~3%的NaOH溶液进行去除),得到所需的电镀图形。
对以下几个因素进行考察:光刻胶形貌的陡直度(涂布完成后,用镭射激光对光刻胶表面进行固化,需要被显影去除的部分,不会被镭射激光固化),光刻胶图形的角度越接近90°越佳;电镀铜后观察胶面是否开裂或渗镀,出现开裂和/或渗镀现象均为不合格;电镀去胶后,观察是否有残留。
测试结果如下表2:
表2
试例 | 光刻胶图形角度 | 电镀后检查 | 去胶干净层度 |
实施例1 | 86.2° | 无开裂无渗镀 | 干净 |
实施例2 | 83.1° | 无开裂无渗镀 | 干净 |
实施例3 | 80.5° | 无开裂无渗镀 | 干净 |
对比例1 | 73.4° | 渗镀 | 残留 |
对比例2 | 72.3° | 渗镀 | 残留 |
对比例3 | 71° | 开裂、渗镀 | 残留 |
由表2可知,实施例1~3采用实施例1中制备的粘结剂聚合物作为光刻胶树脂,并与光反应性单体、光引发剂、交联剂、流平剂以及溶剂混合制备得到的光刻胶,其陡直度均高于80°,且实施例1中制备的光刻胶在上述实验中,测试的陡直度可达86.2°;而采用市售的改性丙烯酸树脂作为光刻胶树脂制备得到的光刻胶,在上述性能测试中,其陡直度均小于75°。
此外,将实施例1~3制备的光刻胶用于电镀铜工艺中,在电镀铜后,胶层表面无开裂或渗镀现象,且经NaOH溶液浸泡即可去胶,并且无残胶现象;而采用对比例1、2制备的光刻胶,在电镀铜后虽未发现开裂现象,但出现了渗镀,并且该胶层经NaOH溶液浸泡后无法去除,仍在基底表面有残留。采用低分子量的光刻胶树脂制备的对比例3中的光刻胶进行电镀铜工艺,电镀后可观察到较为明显的开裂以及渗镀现象,且经NaOH溶液浸泡后太阳能电池表面存在明显的残胶。
除上述实施例及对比例外,本发明还提供了一种高分子量的粘结剂聚合物(在实施例1的基础上,延长聚合反应时间制备得到,重均分子量~10000),并与其它组分(其它组分与实施例1相同)混合制备得到光刻胶,采用该光刻胶用于太阳能电池片铜删的制备,虽未发现开裂、渗镀现象,但胶层不易去除,在一定程度上降低了制备效率。
以上所述实施例仅是为充分说明本发明而所举的较佳的施例,本发明的保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换,均在本发明的保护范围之内。本发明的保护范围以权利要求书为准。
Claims (10)
1.一种用于HJT太阳能电池铜栅制备的光刻胶,其特征在于,所述光刻胶包含按重量份数计的以下组分:粘结剂聚合物30-60份、光反应性单体10-45份、光引发剂1-5份;
所述粘结剂聚合物由丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯和甲基丙烯酸环氧丙酯在引发剂以及溶剂存在下通过自由基聚合得到,所述丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯、甲基丙烯酸环氧丙酯的摩尔比为1:1-1.2:0.8-1.1:0.9-1.1:1-1.2;
所述粘结剂聚合物的重均分子量大于6000。
2.根据权利要求1所述的光刻胶,其特征在于,所述丙烯酸、异戊二烯、甲基丙烯酸、甲基丙烯酸六氟异丙酯、甲基丙烯酸环氧丙酯的摩尔比为1:1.1:1:1:1.1;所述引发剂为偶氮二异丁腈,所述溶剂为丙二醇甲醚醋酸酯;所述自由基聚合的反应温度为70-90,反应时间为6-10h。
3.根据权利要求1所述的光刻胶,其特征在于,所述粘结剂聚合物的重均分子量为6000-9000,分子量分布为1.3-1.7。
5.根据权利要求4所述的光刻胶,其特征在于,所述光反应性单体选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸-2-羟基甲酯、丙烯酸-2-羟基乙酯、丙烯酸-2-羟基丙酯、丙烯酸-2-羟基丁酯中的一种或多种。
6.根据权利要求1所述的光刻胶,其特征在于,所述光引发剂选自苯偶姻类、安息香醚类、二苯甲酮类、米氏酮类、苯乙酮类、吖啶类、蒽醌类、缩酮类、有机卤化物类、重氮萘醌类、有机过氧化物类、硫醇类、噻唑酮类、苯基膦氧类、六芳基咪唑类、香豆素类、噁唑类、吡唑啉类或三芳基胺类化合物中的一种或多种。
7.根据权利要求1所述的光刻胶,其特征在于,所述光刻胶还包含交联剂、流平剂、表面活性剂、阻聚剂、稳定剂、分散剂、增塑剂、染色剂中的一种或多种;所述交联剂为二甲基丙烯酸乙二醇酯和/或双三羟甲基丙烷三丙烯酸酯;所述流平剂为迪高。
8.根据权利要求1所述的光刻胶,其特征在于,所述光刻胶还包含溶剂,所述溶剂甲醇、乙醇、丙醇、丁醇、丙酮、丁酮、N-甲基2-吡咯烷酮、甲基乙基酮、乙二醇单甲醚、乙二醇单乙醚、乙二醇单丙醚、乙二醇单丁醚、甲苯、N,N’-二甲基甲酰胺、丙二醇单甲醚、二甲基亚砜、二乙基亚砜、苯酚、邻甲酚、间甲酚、对甲酚、二甲苯酚、卤代苯酚、邻苯二酚、四氢呋喃、二恶烷、二氧戊环、环丙二醇甲醚、四乙二醇二甲醚、γ-丁内酯、六甲基邻酰胺、丙二醇甲醚醋酸酯中的一种或多种。
9.根据权利要求1所述的光刻胶,其特征在于,所述光刻胶包含按重量份数计的以下组分:粘结剂聚合物30-40份、光反应性单体15-30份、光引发剂2-4份,交联剂1~3份、流平剂0.5~1.5份以及溶剂100~150份。
10.一种权利要求1~9所述光刻胶的制备方法,其特征在于,将光刻胶中各组分根据配方量混合均匀,过滤后得到所述光刻胶。
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