CN114664475B - 一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料及其制备方法 - Google Patents
一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料及其制备方法 Download PDFInfo
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Abstract
一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料及其制备方法,技术领域涉及一种太阳能电池用正面银浆料及其制备方法。本发明的目的是要解决现有制备晶硅太阳能电池导电浆料使用的有机载体中粘结剂、触变剂在电池片烧结后分解残余灰分较多,溶剂易析出,最终导致制备的太阳能电池片拉力水平低和太阳能电池的光电转换效率低的问题。一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料中粘结剂为聚5‑羟基‑2‑戊烯酸乙酯,触变剂为季戊四醇四(9‑氨基‑10‑羟基十八碳酸)酯,分散剂为聚5‑(N,N‑二甲基胺基)‑1,4‑戊二醇单三乙胺醚。本发明可获得一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料。
Description
技术领域
所述技术领域涉及一种太阳能电池用正面银浆料及其制备方法。
背景技术
有机载体作为晶硅太阳能电池导电浆料中的重要辅助成分,其本身对电池片的导电性能并无直接贡献,在银浆料中的含量仅为7%~12%,远小于导电功能相银粉的含量,但是却对银浆料的印刷性和光电转换效率起着至关重要的作用。有机载体主要由溶剂、粘结剂、防流挂剂和润湿剂等成分构成,它们分别赋予银浆料体系以流动性能、粘结性、“一触即变”功能、以及分散性,使得银粉、玻璃粉等粉体材料能在多组分液体中得到较好分散的同时实现对外界施加的剪切应力或剪切速率的快速响应。此外,一种好的有机载体还可保障被载体包裹的粉体能顺利以流体状态印刷于硅基片上,为电极栅线的塑形以及电池内部金属化的进行提供必要的辅助作用。基于太阳能电池银浆料对黏合性、触变性、稳定存储性能、柔韧性、润湿流平性、成膜增塑性、印刷润滑过网性以及外观性状等诸多要求,有机载体中还可以添加其他助剂,包括消泡剂、增塑剂、表面活性剂、偶联剂、润滑剂以及成膜助剂等。
尽管载体中成分和功能多样,但是其与银粉和玻璃粉轧制的浆料却存在一些较难克服的问题,如:
(1)、粘结剂含量问题:为使浆料具有合适的粘度,载体中需添加4%-10%的粘结剂,添加量较低时无法保证浆料在丝网印刷后电极栅线的大高宽比,栅线银浆呈过流平态,栅线边缘规整度较差,电池片受光面积小,导入和流出电子少,严重制约了光电转换效率的提升;粘结剂添加量较高时,因粘结剂本身并不具备导电性能,其在电池片烧结后分解残余灰分较多,对电子在栅线中的顺利流动具有一定的阻碍影响,使得电极栅线与硅片的接触电阻增大,不利于填充因子的提高。
(2)、触变性问题:触变剂一般选择氢化蓖麻油、聚酰胺蜡,气相二氧化硅、有机膨润土等固体,它在提高体系“一触即变”性能的同时也具有增加浆料粘稠度的作用,在电池片烧结后同样存在灰分残余。在四种常见触变剂中,聚酰胺蜡对浆料触变性影响最大,往往只需添加少量即可达到明显的提升触变效果,但需要注意的是,聚酰胺蜡作为一种具有酰胺基团,即-CO-NH2的高分子缩聚物,在较高温度下极易水解分解出NH3,造成聚酰胺蜡结构被破坏,对应地其提升触变的能力也会大打折扣。
(3)、溶剂析出问题:银浆料作为一种多相悬浮体系,其固含量一般≥90%,混合液相和两种固相间必然存在密度差异,这就直接导致了导电浆料体系的不均匀性,直观表现为银粉和玻璃粉在载体中沉降,即溶剂析出,浆料表层出现有别于浆料内部及下层的油性液体。根据斯托克斯经验公式,固体粒子沉降速率v=2gr2(ρs-ρl)/(9η)(其中,g为重力加速度,r为固体粒子半径,ρs、ρl分别为固液体密度,η为流体粘度)可知:①、银粉、玻璃粉粒径越大,粒子沉降越快;②、浆料粘度越大,粒子沉降越慢。尽管粉体粒径及含量属于可控变量,但对于导电浆料而言,该经验公式只是基于恒温、载体中溶剂不挥发、粉体球形粒径具有较高一致性、粉体表面光滑且颗粒间互不碰撞的理想条件的前提下成立,在实际研发及生产中,还需加入具有特有界面活性,兼具亲水基和亲油基的分散剂以使固体颗粒表面得到充分有效润湿和分散,防止轧浆后新生表面快速键合,防止颗粒聚集导致的快速沉降,有效改善载体中溶剂析出问题,提高体系稳定性。
发明内容
本发明的目的是要解决现有制备晶硅太阳能电池导电浆料使用的有机载体中粘结剂、触变剂在电池片烧结后分解残余灰分较多,溶剂易析出,最终导致制备的太阳能电池片拉力水平低和太阳能电池的光电转换效率低的问题,而提供一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料及其制备方法。
一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料按重量份数由85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体制备而成;
所述的有机载体按重量份数由72份~86份溶剂、4份~10份粘结剂、2份~5份触变剂、0.5份~1.5份分散剂、2份~4份塑形剂、5份~9份偶联剂、3份~4份消泡剂和0.2份~0.6份助剂组成;
所述的粘结剂为聚5-羟基-2-戊烯酸乙酯;
所述的触变剂为季戊四醇四(9-氨基-10-羟基十八碳酸)酯;
所述的分散剂为聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚。
一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料的制备方法,是按以下步骤完成的:
一、称料:
按重量份数称取85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体;
二、混合:
将步骤一中称取的银粉、玻璃粉和有机载体混合均匀,然后经三辊机轧制,再使用400目~600目筛网过滤,得到细度小于5μm的低接触电阻且高光电转换效率的太阳能电池用正面银浆料。
本发明的原理及优点:
一、本发明提供了一种粘结性能优异、烧结灰分残余少,电极栅线平滑无外挂,体系稳定的低接触电阻、高光电转换效率的太阳能电池用银浆料;为达到该目的,本发明继续提供了有机载体中使用的粘结剂、触变剂及分散剂的有机合成方法;本发明制备的粘结剂、触变剂及分散剂分别具有分子间缠绕程度较大、印刷烧结后灰分残余少,可提供较多氢键受体和氢键供体,赋予了化合物多点锚固的特点;此外,本发明简化了粘结剂、触变剂及分散剂的制备过程,防止有机合成中因反应线路较长、步骤繁杂导致的副反应较多,进而导致的产率低下和原子利用率不高的问题,同时保证了产物的纯度,避免了多种试剂加入后杂质的引入及提纯不完全的问题;
二、本发明制备的粘结剂具有以下优点:①、聚合物主链中的一个H原子由-CH2CH2OH支链取代,对粘结剂的粘结性能具有显著增强效果;②、-CH2CH2OH链段的引入,使得该高分子聚合物具有更大的空间位阻和更多数量的氢键供体及氢键受体,聚酯树脂的活性得到显著提升;③、该粘结剂经高温烧结后灰分残余较少,对电极栅线中电子的顺利传导影响较小;
三、本发明制备的触变剂具有以下优点:①、选用羟基氨这种特殊化学试剂对(Z)-9-十八碳烯酸(即油酸)中的不饱和双键进行断键加成,同时引入了氨基和羟基,相比于一般只引入单一氨基或羟基的粘结剂而言,本发明制备的触变剂具有成倍的氢键结合位点,可以提供更加致密的三维网状空间结构;②、该触变剂中含有四份子油酸的长支链烷基结构,亲油性、空间缠绕能力以及稳定性能显著增强;
四、本发明制备的分散剂具有以下优点:①、合成路径较短,条件温和,产物的原子利用率达到100 %,且具有较高的收率和纯度;②、α-四氢呋喃甲醛通过与胺类化合物二乙胺加成还原,向环醚化合物引入了-N(CH2CH3)2链段,它与二乙基乙醇胺中的-N(CH2CH3)2一致,属于胺类锚固基团,即在环醚化合物—溶剂化链中直接引入锚固基团,经聚合后产物对固体颗粒表面进行多点锚固,吸附能力显著提高;
五、通过本发明提供的有机载体中的粘结剂、触变剂和分散剂这三种成分,制备的有机载体经轧制浆料、丝网印刷后,最终得到的电池片后具有优异的栅线形貌和电化学性能;
六、使用本发明制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料制备的银栅线的焊接拉力为3.95N~4.2N;
七、使用本发明制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池的光电转换效率为22.8%~22.87%。
本发明可获得一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料。
附图说明
图1为实施例1制备的粘结剂的TG-DSC图;
图2为实施例2制备的触变剂的TG-DSC图;
图3为实施例3制备的分散剂的TG-DSC图;
图4为使用实施例4制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图5为使用实施例5制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图6为使用实施例6制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图7为使用实施例7制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图8为使用实施例8制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图9为使用实施例9制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图;
图10为采用市售银浆料丝网印刷的太阳能电池在烧结过程中玻璃粉飘散的3D显微镜图。
具体实施方式
以下实施例进一步说明本发明的内容,但不应理解为对本发明的限制。在不背离本发明实质的情况下,对本发明方法、步骤或条件所作的修改和替换,均属于本发明的范围。
具体实施方式一:本实施方式一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料按重量份数由85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体制备而成;
所述的有机载体按重量份数由72份~86份溶剂、4份~10份粘结剂、2份~5份触变剂、0.5份~1.5份分散剂、2份~4份塑形剂、5份~9份偶联剂、3份~4份消泡剂和0.2份~0.6份助剂组成;
所述的粘结剂为聚5-羟基-2-戊烯酸乙酯;
所述的触变剂为季戊四醇四(9-氨基-10-羟基十八碳酸)酯;
所述的分散剂为聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚。
具体实施方式二:本实施方式与具体实施方式一不同点是:所述的银粉为高振实密度球形小粒径银粉,振实密度为6.0g/cm3~6.5g/cm3,高振实密度球形小粒径银粉的粒径D50为0.4μm~1.5μm,D100≤2.8μm。其它步骤与具体实施方式一相同。
具体实施方式三:本实施方式与具体实施方式一或二之一不同点是:所述的玻璃粉为高拉力无铅玻璃粉,该玻璃粉按重量份数由30份~45份TeO2、15份~32份Bi2O3、12份~20份B2O3、1份~5份SiO2、0~1份CaO、1份~2份MgO、1.5份~3份ZnO、1份~1.5份Li2O、0.4份~1份Al2O3、5份~10份ZrO2、3份~5份MoO3、2份~4份PtO2、1.5份~3份SrO、0.5份~2份WO3、1份~3份V2O5、0~1份Nb2O5和0~1份ReO2组成。其它步骤与具体实施方式一或二相同。
具体实施方式四:本实施方式与具体实施方式一至三之一不同点是:所述的溶剂为异丙醇、醇酯十二、己二酸二异辛酯、丙二醇苯醚、丁基卡必醇醋酸酯、二乙二醇二丁醚和戊二酸二甲酯中的一种或几种;所述的塑形剂为对苯二甲酸二异丁酯、邻苯二甲酸二环己酯、邻苯二甲酸二仲辛酯、烷基磺酸苯酯和环氧大豆油中的一种或几种。其它步骤与具体实施方式一至三相同。
具体实施方式五:本实施方式与具体实施方式一至四之一不同点是:所述的偶联剂为氨基硅烷、乙烯基硅烷、甲基丙烯酰氧基硅烷、烷基硅烷、环氧硅烷、异丙基二油酸酰氧基钛酸酯和三异硬酯酸钛酸异丙酯中的一种或几种;所述的消泡剂为高级醇消泡剂、聚醚消泡剂、有机硅消泡剂、聚醚改性聚硅氧烷有机硅消泡剂中的一种或几种;所述的高级醇消泡剂为PEG-400;所述的助剂为MT-903,购买自佛山鸿昶新材料有限公司。其它步骤与具体实施方式一至四相同。
具体实施方式六:本实施方式与具体实施方式一至五之一不同点是:所述的聚5-羟基-2-戊烯酸乙酯是按以下步骤制备的:
一、首先使用氮气排除反应容器Ⅰ中的气体,加入催化剂过氧化氢,然后在氮气气氛保护下加入丙炔酸,再通入HBr气体,室温下反应40min~60min,抽滤、干燥,得到反应产物Ⅰ;
步骤一中所述的HBr气体的物质的量与过氧化氢的体积之比为(1mol~1.5mol):46mL;
步骤一中所述的HBr气体与丙炔酸的物质的量之比为(1~1.5):1;
二、将反应产物Ⅰ加入到反应容器Ⅱ内,然后加入无水乙醇,水浴加热至75℃,再在75℃下反应90min,回收产物并抽滤、再于45℃~55℃烘箱内烘干30min,得到反应产物Ⅱ;
步骤二中所述的反应产物Ⅰ与无水乙醇的物质的量比为1:1;
三、将锌屑静置于无水***中充分浸润20min~40min,向反应容器Ⅲ中通入氮气,将反应产物Ⅱ加入到反应容器Ⅲ中,并向反应容器Ⅲ中加入润湿的锌屑和无水***,再加热至45℃,在45℃下恒温回流2h~3h,得到反应产物Ⅲ;
步骤三中所述的锌屑与步骤一中所述的丙炔酸的摩尔比为1:1;
步骤三中所述的锌屑的物质的量与无水***的体积比为(0.2mol~0.5mol):78mL;
四、向反应产物Ⅲ中通入环氧乙烷气体,室温下反应1h~1.5h,再加入TiCl4/MgCl2催化剂,加热至80℃,在80℃下反应6h,过滤,干燥,得到聚5-羟基-2-戊烯酸乙酯;
步骤四中所述的环氧乙烷气体与步骤三中所述的锌屑的摩尔比为(2~2.5):1。其它步骤与具体实施方式一至五相同。
具体实施方式七:本实施方式与具体实施方式一至六之一不同点是:所述的季戊四醇四(9-氨基-10-羟基十八碳酸)酯是按以下步骤制备的:
一、制备季戊四醇:
(1)、向反应容器内加入乙醇钠,以提供碱性反应环境,再通入8min~14min氮气,然后在氮气保护下加入甲醛和乙醛,再在85℃下恒温反应1.5h,回收产物并烘干,得到反应产物Ⅰ;
步骤一(1)中所述的甲醛和乙醛的摩尔比为(3~3.5):1;
(2)、向反应容器内加入乙醇钠,以提供碱性反应环境,然后加入反应产物Ⅰ和甲醛,再加热至70℃,并在70℃下恒温反应2h,抽滤、烘干,得到季戊四醇;
步骤一(2)中所述的甲醛与步骤一(1)中所述的乙醛的摩尔比为1:1;
二、向反应容器内通入10min氮气,再在氮气保护下加入油酸、羟氨和V2O5催化剂,室温下反应8h,抽滤、烘干,得到油酸羟氨化产物;
步骤二中所述的羟氨与油酸的摩尔比为1:1;
三、向反应容器内通入10min氮气,再在氮气保护下加入季戊四醇、油酸羟氨化产物和二氯亚砜催化剂,再加热至60℃,在60℃下反应2.5h,抽滤,烘干,得到季戊四醇四(9-氨基-10-羟基十八碳酸)酯;
步骤三中所述的季戊四醇与油酸羟氨化产物的摩尔比为1:4。其它步骤与具体实施方式一至六相同。
本实施方式中触变剂为季戊四醇四(9-氨基-10-羟基十八碳酸)酯,结构式为
该触变剂具有较多的氢键供体和氢键受体,可通过次价力使浆料中各组分形成庞大紧密的空间三维网状结构;在电池片栅线印刷后的烧结阶段,栅线边缘溶剂挥发更快,引起表面张力不均,栅线中部溶剂易移向边缘,进而带动银粉与玻璃粉向边缘的移动,不利于电极高宽比的提高;若形成氢键程度较高,各分子在三维网状结构中的可活动空间较小,在溶剂挥发过程中紧密的触变网络结构能有效阻止溶剂的横向移动,大大减缓了浆料流挂程度,同时栅线边缘平整度也会提高;该触变剂是以季戊四醇和(Z)-9-十八碳烯酸(即油酸)为原料合成的,反应方程式如下:
具体实施方式八:本实施方式与具体实施方式一至七之一不同点是:所述的聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚是按以下步骤制备的:
一、制备叔氨修饰的五元环醚:
(1)、向反应容器内加入金属Ni作为催化剂,然后将反应容器在25℃下水浴恒温,加入α-呋喃甲醛,再向反应容器内持续通入H2,反应进行3 h后停止通入H2,关闭水浴***,抽滤,烘干,得到α-四氢呋喃甲醛;
步骤一(1)中所述的H2与α-呋喃甲醛的摩尔比为(3~10):1;
(2)、将α-四氢呋喃甲醛加入到反应容器内,然后加入二乙胺和氰基硼氢化钠,再加热至100℃,在100℃下反应2.5h,抽滤,烘干,得到叔氨修饰的五元环醚;
步骤一(2)中所述的α-四氢呋喃甲醛与二乙胺的摩尔比为1:1;
步骤一(2)中所述的α-四氢呋喃甲醛与氰基硼氢化钠的摩尔比为1:1.25;
二、向反应釜内依次加入催化剂KOH、叔氨修饰的五元环醚和二乙基乙醇胺,在130℃和0.35 MPa的反应条件下持续反应5h,再过滤,干燥,得到聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚;
步骤二中所述的二乙基乙醇胺与叔氨修饰的五元环醚的摩尔比为1:(63~95)。其它步骤与具体实施方式一至七相同。
本实施方式中分散剂为聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚,结构式为;分散剂是一种使颗粒表面迅速润湿的特殊表面活性剂,有机载体中的分散剂具有提高导电浆料加工性能、流变特性和印刷性能的作用。该分散剂属于强极性聚醚型分散剂,与传统分散剂相比,该分散剂具有更大的分子量和碳链长度,在结构上具备更多的官能性锚固基团,这些特征为该分散剂提供了更大的空间位阻和更多的氢键结合位点,以实现优异的稳定效果;该分散剂由锚固基团和溶剂化链两部分组成,其中,前者主要是通过氢键、共价键、范德华力等作用力与固体颗粒表面牢固吸附,有效防止了分散剂与较低极性固体颗粒的脱附,而溶剂化链则能在分散介质中自由无序伸展,包裹固体颗粒,为其提供保护层。本实施方式的聚醚型分散剂选定二乙基乙醇胺为锚固基团,由经叔氨修饰的五元环醚提供溶剂化链,反应方程式如下:
具体实施方式九:本实施方式与具体实施方式一至八之一不同点是:一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料的制备方法,是按以下步骤完成的:
一、称料:
按重量份数称取85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体;
二、混合:
将步骤一中称取的银粉、玻璃粉和有机载体混合均匀,然后经三辊机轧制,再使用400目~600目筛网过滤,得到细度小于5μm的低接触电阻且高光电转换效率的太阳能电池用正面银浆料。其它步骤与具体实施方式一至八相同。
具体实施方式十:本实施方式是所述的玻璃粉是按以下步骤制备的:
①、按重量份数称取30份~45份TeO2、15份~32份Bi2O3、12份~20份B2O3、1份~5份SiO2、0~1份CaO、1份~2份MgO、1.5份~3份ZnO、1份~1.5份Li2O、0.4份~1份Al2O3、5份~10份ZrO2、2份~5份MoO3、2份~4份PtO2、1.5份~3份SrO、0.5份~2份WO3、1份~3份V2O5、0~1份Nb2O5和0~1份ReO2,得到原料;
②、将原料加入到玛瑙研钵中研磨25min~50min,再放入温度为50℃~70℃的干燥箱干燥30min~50min,得到干燥的原料;
③、将干燥的原料转至刚玉坩埚中,再在1100℃~1300℃的条件下煅烧30min~60min,得到玻璃液;
④、将玻璃液倒入去离子水中淬火处理,冷却至室温,取出粗制玻璃颗粒并烘干;
⑤、将烘干的粗制玻璃颗粒加入到球磨机中,使用无水乙醇作为球磨助剂进行球磨,球磨后使用200目~400目的筛网进行过筛处理,得到玻璃粉;
步骤⑤中所述的玻璃粉的粒径为:D50:0.8~2.2μm,D90:2.5~3.0μm,软化点为480℃~525℃;
所述的有机载体是按以下步骤制备的:
步骤(1)、按重量份数称取72份~86份溶剂、4份~10份粘结剂、2份~5份触变剂、0.5份~1.5份分散剂、2份~4份塑形剂、5份~9份偶联剂、3份~4份消泡剂和0.2份~0.6份助剂,得到试剂;
步骤(2)、将试剂在温度为75℃~85℃和搅拌速度800r/min~1500r/min的条件下搅拌2.5h~3.5h,再使用300目~600目筛网过滤,冷却至室温,得到有机载体。
采用以下实施例验证本发明的有益效果:
实施例1:粘结剂聚5-羟基-2-戊烯酸乙酯是按以下步骤制备的:
一、首先使用氮气排除反应容器Ⅰ中的气体,加入催化剂过氧化氢,然后在氮气气氛保护下加入丙炔酸,再通入HBr气体,室温下反应50min,抽滤、干燥,得到反应产物Ⅰ;
步骤一中所述的HBr气体的物质的量与过氧化氢的体积之比为1.5mol:46mL;
步骤一中所述的HBr气体与丙炔酸的物质的量之比为1:1;
二、将反应产物Ⅰ加入到反应容器Ⅱ内,然后加入无水乙醇,水浴加热至75℃,再在75℃下反应90min,回收产物并抽滤、再于50℃烘箱内烘干30min,得到反应产物Ⅱ;
步骤二中所述的反应产物Ⅰ与无水乙醇的物质的量比为1:1;
三、将锌屑静置于无水***中充分浸润30min,向反应容器Ⅲ中通入氮气,将反应产物Ⅱ加入到反应容器Ⅲ中,并向反应容器Ⅲ中加入润湿的锌屑和无水***,再加热至45℃,在45℃下恒温回流2.5h,得到反应产物Ⅲ;
步骤三中所述的锌屑与步骤一中所述的丙炔酸的摩尔比为1:1;
步骤三中所述的锌屑的物质的量与无水***的体积比为0.3mol:78mL;
四、向反应产物Ⅲ中通入环氧乙烷气体,室温下反应1h~1.5h,再加入TiCl4/MgCl2催化剂,加热至80℃,在80℃下反应6h,过滤,干燥,得到聚5-羟基-2-戊烯酸乙酯;
步骤四中所述的环氧乙烷气体与步骤三中所述的锌屑的摩尔比为2.2:1。
实施例2:触变剂季戊四醇四(9-氨基-10-羟基十八碳酸)酯是按以下步骤制备的:
一、制备季戊四醇:
(1)、向反应容器内加入乙醇钠,以提供碱性反应环境,再通入14min氮气,然后在氮气保护下加入甲醛和乙醛,再在85℃下恒温反应1.5h,回收产物并烘干,得到反应产物Ⅰ;
步骤一(1)中所述的甲醛和乙醛的摩尔比为3.2:1;
(2)、向反应容器内加入乙醇钠,以提供碱性反应环境,然后加入反应产物Ⅰ和甲醛,再加热至70℃,并在70℃下恒温反应2h,抽滤、烘干,得到季戊四醇;
步骤一(2)中所述的甲醛与步骤一(1)中所述的乙醛的摩尔比为1:1;
二、向反应容器内通入10min氮气,再在氮气保护下加入油酸、羟氨和V2O5催化剂,室温下反应8h,抽滤、烘干,得到油酸羟氨化产物;
步骤二中所述的羟氨与油酸的摩尔比为1:1;
三、向反应容器内通入10min氮气,再在氮气保护下加入季戊四醇、油酸羟氨化产物和二氯亚砜(催化剂),再加热至60℃,在60℃下反应2.5h,抽滤,烘干,得到季戊四醇四(9-氨基-10-羟基十八碳酸)酯;
步骤三中所述的季戊四醇与油酸羟氨化产物的摩尔比为1:4。
实施例3:分散剂聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚,是按以下步骤制备的:
一、制备叔氨修饰的五元环醚:
(1)、向反应容器内加入金属Ni作为催化剂,然后将反应容器在25℃下水浴恒温,加入α-呋喃甲醛,再向反应容器内持续通入H2,反应进行3 h后停止通入H2,关闭水浴***,抽滤,烘干,得到α-四氢呋喃甲醛;
步骤一(1)中所述的H2与α-呋喃甲醛的摩尔比为5:1;
(2)、将α-四氢呋喃甲醛加入到反应容器内,然后加入二乙胺和氰基硼氢化钠,再加热至100℃,在100℃下反应2.5h,抽滤,烘干,得到叔氨修饰的五元环醚;
步骤一(2)中所述的α-四氢呋喃甲醛与二乙胺的摩尔比为1:1;
步骤一(2)中所述的α-四氢呋喃甲醛与氰基硼氢化钠的摩尔比为1:1.25;
二、向反应釜内依次加入催化剂KOH、叔氨修饰的五元环醚和二乙基乙醇胺,在130℃和0.35 MPa的反应条件下持续反应5h,再过滤,干燥,得到聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚;
步骤二中所述的二乙基乙醇胺与叔氨修饰的五元环醚的摩尔比为1:75.56。
对实施例1~3合成的三种有机物进行TG-DSC测试:该测试在空气气氛下进行,升温速度为10 ℃/min,终止温度为500 ℃,测试曲线见图1~3所示:图1~3中,横坐标为温度,由加热炉打开、自然冷却到的室温25℃左右为加热起始温度,500℃的设定温度为升温终点;纵坐标为两个响应变量-重量变化及坩埚内热量变化,分别对应TG曲线和DSC曲线,其中TG曲线反映了粘结剂、触变剂、分散剂随温度和时间变化的失重情况,是物质在一定高温下分解能力的度量,而DSC曲线则表现了三种测试样品随时间在不同温度下吸热、放热速率,凸起峰和凹陷峰分别对应体系热焓的增加和减少;测试结果见表1所示;
从表1可知:在500 ℃程序升温终止温度下,由本发明制备的粘结剂、触变剂以及分散剂均能基本分解完全。三种成分分别在245.46℃,159.97℃,127.41℃下开始少量分解;当加热炉炉腔内温度分别达到356.34℃,314.74℃,273.08℃时,坩埚内仅有20%残余,之后随温度继续上升,残余量逐渐减少;三种固体成分均能满足电池片烧结后栅线内不导电灰分残余少的要求,对降低接触电阻从而提高转换因子具有积极影响。
实施例4:一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料的制备方法是按以下步骤完成的:
一、制备玻璃粉:
①、按重量份数称取38份TeO2、20份Bi2O3、15份B2O3、2.5份SiO2、0.8份CaO、1.5份MgO、2份ZnO、1.2份Li2O、0.6份Al2O3、7份ZrO2、2.5份MoO3、3份PtO2、2.4份SrO、1份WO3、1.7份V2O5、0.5份Nb2O5和0.3份ReO2,得到原料;
②、将原料加入到玛瑙研钵中研磨30min,再放入温度为65℃的干燥箱干燥45min,得到干燥的原料;
③、将干燥的原料转至刚玉坩埚中,再在1250℃的条件下煅烧50min,得到玻璃液;
④、将玻璃液倒入去离子水中淬火处理,冷却至室温,取出粗制玻璃颗粒并烘干;
⑤、将烘干的粗制玻璃颗粒加入到球磨机中,使用无水乙醇作为球磨助剂进行球磨,球磨后使用360目的筛网进行过筛处理,得到玻璃粉;
步骤⑤中所述的玻璃粉的粒径为:D50:0.8~2.2μm,D90:2.5~3.0μm,软化点为480℃~525℃;
二、制备有机载体:
步骤(1)、按质量百分比称取20.5%醇酯十二、15%丙二醇苯醚、12.5%丁基卡必醇醋酸酯、18%二乙二醇二丁醚、10%戊二酸二甲酯、5.2%实施例1制备的粘结剂聚5-羟基-2-戊烯酸乙酯、4%实施例2制备的触变剂季戊四醇四(9-氨基-10-羟基十八碳酸)酯、0.8%实施例3制备的分散剂聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚、3%对苯二甲酸二异丁酯、7%硅烷偶联剂KH-570、3.6%PEG-400和0.5%触变流变控制剂MT-903,得到试剂;
步骤(2)、将试剂在温度为80℃和搅拌速度1200r/min的条件下搅拌3h,再使用450目筛网过滤,冷却至室温,得到有机载体;
三、称料:
按重量份数称取89.8份银粉、2.5份玻璃粉和7.7份有机载体;
步骤二中所述的银粉为DowaAG-3-8F,购买自DOWA ELECTRONICS MATERIALS CO.,LTD.公司;振实密度为6.0g/cm3~6.5g/cm3,D50为0.4μm~1.5μm,D100≤2.8μm;
四、混合:
将步骤三中称取的银粉、玻璃粉和有机载体混合均匀,然后经三辊机轧制,再使用600目筛网过滤,得到细度小于5μm的低接触电阻且高光电转换效率的太阳能电池用正面银浆料。
实施例5~9与实施例4的不同点是有机载体中各物质的含量不同,具体见表2所示;
实施例4~9的有机载体体系中添加有聚乙二醇PEG-400作消泡剂,PEG-400除具有消泡性能以外,还可提高载体和浆料的粘度、触变值。为确保栅线边缘较高平整度,有机载体中还添加了0.4 %的触变流变控制剂MT-903,以得到平滑、规整的电极栅线。
采用一款市售银浆料、实施例4~9制备的低接触电阻且高光电转换效率的太阳能电池用正面银浆料通过丝网印刷印在电池片(硅片)上,通过烧结炉烧结成电池片,最高烧结温度875℃;使用3D显微镜观测形貌,见图4~图10所示;在图4中,栅线平滑且栅线线形较为规整,边缘基本无流挂,但线宽相对较大,经3D测试后得到的高宽比在6个实施例中较小;在图5中,栅线线宽明显较图4小,但栅线规整度略差于图4中栅线,可观察到较为明显的栅线凸起;在图6中,栅线线宽较大,栅线平滑度较高,但边缘略微发虚;在图7中,栅线线宽较小,边缘非常规整无流挂;在图8中,栅线线宽也较小,但能观察到较为明显的凸起,栅线边缘略微发虚,程度稍弱于图6中栅线发虚程度;在图9中,同样可以观察到栅线上轻微凸起,栅线边缘规整度较低且发虚相对明显;在图10中,栅线规整度与图4~9存在差异,栅线较宽,可以观察到凸起,边缘印刷质量不高。
从图4~图10可知:由本发明提供的正银浆料在经丝网印刷工艺后得到的电池片具有优异的栅线形貌:副栅线型完整,无断点、断栅、虚印、漏印现象;栅线边缘平滑且较规整,流挂得到有效改善。其中,实施例7具有更为优异的栅线图形,从图7可知:经过该浆料配方轧制的正银浆料具有更加优异的栅线形貌,说明实施例7中的有机载体组成及质量分数更匹配本发明提供的正银浆料配方,由本发明提供的粘结剂、触变剂及分散剂的含量在该有机载体中分别为5.6%,3.4%,1%时,效果最好。
对得到的电池片依次进行效率测试、高宽比测试、TLM接触电阻测试、EL测试、拉力测试;测试结果见表3所示:
从表3可知:对比一款市售银浆料,本发明提供的正银浆料具有更低的接触电阻、更高的光电转换效率以及较好的焊接拉力。此外,这两种银浆料印刷制得的电池片均具有0.3以上的高宽比,且EL正常,基本无断点断栅现象,说明由本发明提供的正银浆料具有优异的电化学性能,具备一定实际生产价值。
Claims (7)
1.一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料,其特征在于,一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料按重量份数由85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体制备而成;
所述的有机载体按重量份数由72份~86份溶剂、4份~10份粘结剂、2份~5份触变剂、0.5份~1.5份分散剂、2份~4份塑形剂、5份~9份偶联剂、3份~4份消泡剂和0.2份~0.6份触变流变控制剂MT-903组成;
所述的粘结剂为聚5-羟基-2-戊烯酸乙酯,其是按以下步骤制备的:
一、首先使用氮气排除反应容器Ⅰ中的气体,加入催化剂过氧化氢,然后在氮气气氛保护下加入丙炔酸,再通入HBr气体,室温下反应40min~60min,抽滤、干燥,得到反应产物Ⅰ;
步骤一中所述的HBr气体的物质的量与过氧化氢的体积之比为(1mol~1.5mol):46mL;
步骤一中所述的HBr气体与丙炔酸的物质的量之比为(1~1.5):1;
二、将反应产物Ⅰ加入到反应容器Ⅱ内,然后加入无水乙醇,水浴加热至75℃,再在75℃下反应90min,回收产物并抽滤、再于45℃~55℃烘箱内烘干30min,得到反应产物Ⅱ;
步骤二中所述的反应产物Ⅰ与无水乙醇的物质的量比为1:1;
三、将锌屑静置于无水***中充分浸润20min~40min,向反应容器Ⅲ中通入氮气,将反应产物Ⅱ加入到反应容器Ⅲ中,并向反应容器Ⅲ中加入润湿的锌屑和无水***,再加热至45℃,在45℃下恒温回流2h~3h,得到反应产物Ⅲ;
步骤三中所述的锌屑与步骤一中所述的丙炔酸的摩尔比为1:1;
步骤三中所述的锌屑的物质的量与无水***的体积比为(0.2mol~0.5mol):78mL;
四、向反应产物Ⅲ中通入环氧乙烷气体,室温下反应1h~1.5h,再加入TiCl4/MgCl2催化剂,加热至80℃,在80℃下反应6h,过滤,干燥,得到聚5-羟基-2-戊烯酸乙酯;
步骤四中所述的环氧乙烷气体与步骤三中所述的锌屑的摩尔比为(2~2.5):1;
所述的触变剂为季戊四醇四(9-氨基-10-羟基十八碳酸)酯,其是按以下步骤制备的:
一、制备季戊四醇:
(1)、向反应容器内加入乙醇钠,以提供碱性反应环境,再通入8min~14min氮气,然后在氮气保护下加入甲醛和乙醛,再在85℃下恒温反应1.5h,回收产物并烘干,得到反应产物Ⅰ;
步骤一(1)中所述的甲醛和乙醛的摩尔比为(3~3.5):1;
(2)、向反应容器内加入乙醇钠,以提供碱性反应环境,然后加入反应产物Ⅰ和甲醛,再加热至70℃,并在70℃下恒温反应2h,抽滤、烘干,得到季戊四醇;
步骤一(2)中所述的甲醛与步骤一(1)中所述的乙醛的摩尔比为1:1;
二、向反应容器内通入10min氮气,再在氮气保护下加入油酸、羟氨和V2O5催化剂,室温下反应8h,抽滤、烘干,得到油酸羟氨化产物;
步骤二中所述的羟氨与油酸的摩尔比为1:1;
三、向反应容器内通入10min氮气,再在氮气保护下加入季戊四醇、油酸羟氨化产物和二氯亚砜催化剂,再加热至60℃,在60℃下反应2.5h,抽滤,烘干,得到季戊四醇四(9-氨基-10-羟基十八碳酸)酯;
步骤三中所述的季戊四醇与油酸羟氨化产物的摩尔比为1:4;
所述的分散剂为聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚,其是按以下步骤制备的:
一、制备叔氨修饰的五元环醚:
(1)、向反应容器内加入金属Ni作为催化剂,然后将反应容器在25℃下水浴恒温,加入α-呋喃甲醛,再向反应容器内持续通入H2,反应进行3 h后停止通入H2,关闭水浴***,抽滤,烘干,得到α-四氢呋喃甲醛;
步骤一(1)中所述的H2与α-呋喃甲醛的摩尔比为(3~10):1;
(2)、将α-四氢呋喃甲醛加入到反应容器内,然后加入二乙胺和氰基硼氢化钠,再加热至100℃,在100℃下反应2.5h,抽滤,烘干,得到叔氨修饰的五元环醚;
步骤一(2)中所述的α-四氢呋喃甲醛与二乙胺的摩尔比为1:1;
步骤一(2)中所述的α-四氢呋喃甲醛与氰基硼氢化钠的摩尔比为1:1.25;
二、向反应釜内依次加入催化剂KOH、叔氨修饰的五元环醚和二乙基乙醇胺,在130℃和0.35 MPa的反应条件下持续反应5h,再过滤,干燥,得到聚5-(N,N-二甲基胺基)-1,4-戊二醇单三乙胺醚;
步骤二中所述的二乙基乙醇胺与叔氨修饰的五元环醚的摩尔比为1:(63~95)。
2.根据权利要求1所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料,其特征在于,所述的银粉为高振实密度球形小粒径银粉,振实密度为6.0g/cm3~6.5g/cm3,高振实密度球形小粒径银粉的粒径D50为0.4μm~1.5μm,D100≤2.8μm。
3.根据权利要求1所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料,其特征在于,所述的玻璃粉为高拉力无铅玻璃粉,该玻璃粉按重量份数由30份~45份TeO2、15份~32份Bi2O3、12份~20份B2O3、1份~5份SiO2、0~1份CaO、1份~2份MgO、1.5份~3份ZnO、1份~1.5份Li2O、0.4份~1份Al2O3、5份~10份ZrO2、2份~5份MoO3、2份~4份PtO2、1.5份~3份SrO、0.5份~2份WO3、1份~3份V2O5、0~1份Nb2O5和0~1份ReO2组成。
4.根据权利要求1、2或3所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料,其特征在于,所述的溶剂为异丙醇、醇酯十二、己二酸二异辛酯、丙二醇苯醚、丁基卡必醇醋酸酯、二乙二醇二丁醚和戊二酸二甲酯中的一种或几种;所述的塑形剂为对苯二甲酸二异丁酯、邻苯二甲酸二环己酯、邻苯二甲酸二仲辛酯、烷基磺酸苯酯和环氧大豆油中的一种或几种。
5.根据权利要求1、2或3所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料,其特征在于,所述的偶联剂为氨基硅烷、乙烯基硅烷、甲基丙烯酰氧基硅烷、烷基硅烷、环氧硅烷、异丙基二油酸酰氧基钛酸酯和三异硬酯酸钛酸异丙酯中的一种或几种;所述的消泡剂为高级醇消泡剂、聚醚消泡剂、有机硅消泡剂、聚醚改性聚硅氧烷有机硅消泡剂中的一种或几种;所述的高级醇消泡剂为PEG-400。
6.如权利要求1所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料的制备方法,其特征在于,其是按以下步骤完成的:
一、称料:
按重量份数称取85份~95份银粉、1.8份~3.0份玻璃粉和7份~12份有机载体;
二、混合:
将步骤一中称取的银粉、玻璃粉和有机载体混合均匀,然后经三辊机轧制,再使用400目~600目筛网过滤,得到细度小于5μm的低接触电阻且高光电转换效率的太阳能电池用正面银浆料。
7.根据权利要求6所述的一种低接触电阻且高光电转换效率的太阳能电池用正面银浆料的制备方法,其特征在于,所述的玻璃粉是按以下步骤制备的:
①、按重量份数称取30份~45份TeO2、15份~32份Bi2O3、12份~20份B2O3、1份~5份SiO2、0~1份CaO、1份~2份MgO、1.5份~3份ZnO、1份~1.5份Li2O、0.4份~1份Al2O3、5份~10份ZrO2、2份~5份MoO3、2份~4份PtO2、1.5份~3份SrO、0.5份~2份WO3、1份~3份V2O5、0~1份Nb2O5和0~1份ReO2,得到原料;
②、将原料加入到玛瑙研钵中研磨25min~50min,再放入温度为50℃~70℃的干燥箱干燥30min~50min,得到干燥的原料;
③、将干燥的原料转至刚玉坩埚中,再在1100℃~1300℃的条件下煅烧30min~60min,得到玻璃液;
④、将玻璃液倒入去离子水中淬火处理,冷却至室温,取出粗制玻璃颗粒并烘干;
⑤、将烘干的粗制玻璃颗粒加入到球磨机中,使用无水乙醇作为球磨助剂进行球磨,球磨后使用200目~400目的筛网进行过筛处理,得到玻璃粉;
步骤⑤中所述的玻璃粉的粒径为:D50:0.8~2.2μm,D90:2.5~3.0μm,软化点为480℃~525℃;
所述的有机载体是按以下步骤制备的:
步骤(1)、按重量份数称取72份~86份溶剂、4份~10份粘结剂、2份~5份触变剂、0.5份~1.5份分散剂、2份~4份塑形剂、5份~9份偶联剂、3份~4份消泡剂和0.2份~0.6份触变流变控制剂MT-903,得到试剂;
步骤(2)、将试剂在温度为75℃~85℃和搅拌速度800r/min~1500r/min的条件下搅拌2.5h~3.5h,再使用300目~600目筛网过滤,冷却至室温,得到有机载体。
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