CN107138372B - 一种通过表面结晶改善二氧化硅光学特性的方法 - Google Patents
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Abstract
一种通过表面结晶改善二氧化硅光学特性的方法，包含以下步骤：(1)将化学改性后的纳米二氧化硅溶胶颗粒均匀涂于硅片上；(2)将步骤(1)中涂有二氧化硅的硅片在炉子中进行高压惰性气体热处理，热处理温度为100‑1800℃，气体压力为0.1‑6MPa，热处理时间为1‑10h，得到颗粒表面部分结晶的均匀二氧化硅膜层。经过高压惰性气氛快速升降温热处理的二氧化硅膜层，光学特性有所改善，折射率提高且连续可调，可作为太阳能电池梯度折射率减反层的理想材料。该膜层的制备工艺简单，原料成本低，有利于实现大规模工业化生产。
Description
技术领域
本发明属于无机非金属材料领域，具体涉及一种通过表面结晶改善二氧化硅膜层光学特性的方法，特别涉及一种通过高压惰性气氛快速升降温热处理促进二氧化硅颗粒表面结晶的工艺。
背景技术
太阳能是目前为止最为清洁、可持续的能源。2015年，全球光伏新增装机量达36GW，未来几年将继续增加。届时，光伏发电将在极大程度上解决世界能源紧缺的问题。
对于高效太阳能电池，光吸收过程是光电转换的关键的第一步，直接影响光电转换的效率，因此，增加光的吸收，减少光反射对提高太阳能电池转换效率具有重要的意义。一般情况下，当光照射到某一平面样品表面时，会发生光的反射，反射率的大小由样品和外界透明介质的折射率决定。对于普通的抛光硅片，表面反射率高达35％，这意味着，若硅表面不进行任何减反射处理，光从空气中入射到硅电池表面时，将有1/3的光被浪费。因此，我们在空气中和硅片之间增加减反层，来提高光的透过率。
根据光的折射定律，当光线从低折射率介质向高折射率介质传播时，折射角增大。当入射角较大时，则有可能发生全反射，这样光线就可以被更长地锁在低折射率介质内部形成“光池”。因此，若用于制备减反层颗粒的表面的折射率高于颗粒内部，则光线在颗粒内部的停留时间就会延长，光线的利用率得以提高。
相比于单层或双层减反膜，多层减反膜对宽波段的光具有更好的减反效果。在利用多层膜作减反射时，欲达到优异的减反射效果，每层膜的折射率会呈现近连续的变化。由此，人们引入梯度折射率的概念。梯度折射率材料是一种非匀质材料，其组分和结构在材料内部按一定规律连续变化，从而使折射率也相应地呈连续变化。所谓的梯度折射率减反射层，是指由一系列折射率逐渐从入射介质变化到衬底介质的材料所组成的减反射层。
2007年，Xi.J.Q.等利用倾斜气相沉积技术在Si片上制备了5层梯度折射率分布的纳米微结构减反射膜层，实现了非常好的梯度折射率宽带减反射，希望将这种优秀的技术在未来能应用于晶Si太阳能电池片的减反射，但该技术对设备要求严格，成本较高，很难实现工业化生产。因此，低成本、高效率的梯度折射率减反层及减反层材料的制备仍需进一步的探索。
发明内容：
本发明针对二氧化硅膜层作为太阳能电池梯度折射率减反层的材料，提供一种工艺简单、成本较低的连续变折射率的二氧化硅膜层的制备方法，克服了已有技术的缺点，所制得二氧化硅膜层具有良好的均匀性和热稳定性，膜层内颗粒粒度在10-100nm范围内，且使得非晶颗粒的表面存在纳米结晶微区，使光线在颗粒内部的停留时间得以提高，通过调控表面结晶程度可实现二氧化硅膜层的折射率的连续变化。
本发明提出的一种通过表面结晶改善二氧化硅光学特性的方法，包含以下步骤：
(1)将化学改性后的纳米二氧化硅溶胶颗粒均匀涂于硅片上；
(2)将步骤(1)中涂有二氧化硅的硅片在炉子中进行高压惰性气体热处理，热处理温度为100-1800℃，优选1000-1200℃，气体压力为0.1-6MPa，优选4MPa，热处理时间为1-10h，优选1-5h，得到颗粒表面结晶的均匀二氧化硅膜层。
所述步骤(1)中的二氧化硅溶胶颗粒为非晶态二氧化硅，平均粒径为10-100nm，分散性良好，无团聚。
所述步骤(1)中采用坩埚承托硅片，所述坩埚为石墨、氧化铝、氮化硼、碳化硅、石英坩埚中的一种。
所述步骤(2)中的惰性气体为氩气、氮气、氦气中的一种或几种。
所述步骤(2)中的温度优选为100-1500℃。
所述步骤(2)中的热处理时间优选为1-5h。
所述步骤(2)中的热处理过程的升温速率在5-50℃/min之间，降温速率在5-50℃/min之间。
所述步骤(2)中的炉子采用气压热处理炉。
本发明的创新思路在于，采用高压惰性气氛的快速升降温热处理使纳米二氧化硅颗粒表面结晶，防止颗粒间进一步团聚以提高膜层均匀性，同时改善二氧化硅的光学特性。10-100nm的纳米级SiO2颗粒具有很高的表面能，团聚的结合强度很大，一旦团聚，就很难再次被分散。经化学改性后的二氧化硅颗粒在常温下具有良好的分散性，但热稳定性较差。特别是在处于较高的温度下时，与颗粒结合的表面活性剂中的有机成分挥发，颗粒间发生剧烈团聚，分散性急剧恶化，形成二氧化硅的膜层均匀性很差。本发明在高压惰性气氛下对二氧化硅进行热处理，一方面高压惰性气氛和较快的升降温速率可以抑制表面活性剂的挥发，防止颗粒间的团聚；另一方面，热处理也降低了颗粒表面能，甚至使表面部分结晶，可彻底解决团聚问题，提高膜层的均匀性。二氧化硅的折射率介于硅(n＝3.2)和空气(n＝1)之间，是太阳能电池减反层的理想材料，高压惰性气氛的快速升降温热处理也可改善二氧化硅的光学性能。其一，由于二氧化硅颗粒非晶内部的折射率较低，而结晶表面的折射率较高，光线可更多停留在颗粒内部形成“光池”，从而光线的逗留时间也得到延长，提高光线的利用率。其二，由于晶体二氧化硅比非晶的二氧化硅具有更高的折射率，通过调控热处理参数可改变纳米二氧化硅颗粒表面的结晶程度，可得到折射率连续变化的二氧化硅膜层，从而可以作为太阳能电池梯度折射率减反层的理想材料。
本发明与现有技术相比具有以下优点：
(1)采用表面活性剂对纳米二氧化硅进行化学改性，可以使二氧化硅在室温下保持良好的分散性，在后续高压惰性气氛下快速升降温热处理的过程中，表面活性剂具有较慢的挥发速度，抑制了二氧化硅颗粒之间的团聚趋势，提高了膜层的均匀性。
(2)使用10-100nm单分散的纳米二氧化硅溶胶颗粒为原料。一方面，常温下的二氧化硅具有良好的分散性，为后续制得具有良好热稳定性和均匀性、表面结晶的二氧化硅膜层提供了前提。
(3)在高压惰性气氛中对二氧化硅进行热处理，可以抑制表面活性剂挥发速度，防止二氧化硅颗粒间团聚。
(4)采用快速升降温的方式对二氧化硅进行热处理，可以在表面活性剂完全挥发之前达到二氧化硅结晶温度，并迅速实现二氧化硅的表面结晶，防止颗粒整体完全结晶。
(5)本方法生产周期较短，工艺简单，操作方便，且生产成本较低。
(6)按本发明制备的颗粒表面结晶的二氧化硅膜层，具有良好的均匀性和热稳定性。
(7)表面结晶的二氧化硅颗粒形成“光池”，使光线利用率提高；二氧化硅膜层的光学折射率也可以通过调节热处理参数实现连续变化，故可以满足太阳能电池梯度折射率减反层的应用要求。
附图说明
图1：热处理前二氧化硅溶胶颗粒的形貌照片；
图2：热处理前二氧化硅膜层的X射线衍射图谱；
图3：实施例2中热处理后二氧化硅膜层的X射线衍射图谱；
图4：实施例2中热处理后二氧化硅膜层内颗粒的透射电镜照片。
具体实施方式
实施例1
用聚乙二醇对纳米二氧化硅溶胶颗粒进行化学改性，并将溶胶均匀涂于硅片上。将涂有二氧化硅颗粒的硅片置于坩埚中，在炉子中进行热处理，热处理温度为1200℃，炉内气氛为氩气，气体压力为4MPa，热处理时间为5h，热处理的升温速率为10℃/min，降温速率为10℃/min，得到颗粒表面结晶的均匀二氧化硅膜层。
实施例2
用聚乙二醇对纳米二氧化硅溶胶颗粒进行化学改性，并将溶胶均匀涂于硅片上。将涂有二氧化硅颗粒的硅片置于坩埚中，在炉子中进行热处理，热处理温度为1200℃，炉内气氛为氩气，气体压力为4MPa，热处理时间为1h，热处理的升温速率为10℃/min，降温速率为10℃/min，得到颗粒表面结晶的均匀二氧化硅膜层。
对热处理前后的二氧化硅膜层进行折射率测试，测量结果列于表1。
表1高压惰性气氛快速升降温热处理前后二氧化硅膜层的折射率
| 热处理前 | 实施例1 | 实施例2 | |
| 折射率(n) | 1.22 | 1.40 | 1.49 |
上述实施例对本发明的技术方案进行了详细说明。显然，本发明并不局限于所描述的实施例。基于本发明中的实施例，熟悉本技术领域的人员还可据此做出多种变化，但任何与本发明等同或相类似的变化都属于本发明保护的范围。
Claims (8)
1.一种通过表面结晶改善二氧化硅光学特性的方法，其特征在于，包含以下步骤：
(1)将化学改性后的纳米二氧化硅溶胶颗粒均匀涂于硅片上；所述的二氧化硅溶胶颗粒为非晶态二氧化硅，平均粒径为10-100nm，分散性良好，无团聚；
(2)将步骤(1)中涂有二氧化硅的硅片在炉子中进行高压惰性气体热处理，热处理温度为100-1800℃，气体压力为4-6MPa，热处理时间为1-10h，得到颗粒表面部分结晶的均匀二氧化硅膜层；热处理过程的升温速率在10-50℃/min之间，降温速率在10-50℃/min之间。
2.根据权利要求1所述的方法，其特征在于，步骤(1)中采用坩埚承托硅片，所述坩埚为石墨、氧化铝、氮化硼、碳化硅、石英坩埚中的一种。
3.根据权利要求1所述的方法，其特征在于，步骤(2)中所述的惰性气体为氩气、氮气、氦气中的一种或几种。
4.根据权利要求1所述的方法，其特征在于，步骤(2)中所述的温度为1000-1200℃。
5.根据权利要求1所述的方法，其特征在于，步骤(2)中所述的热处理时间为1-5h。
6.根据权利要求1所述的方法，其特征在于，步骤(2)中所述炉子采用气压热处理炉。
7.根据权利要求1所述的方法，其特征在于，步骤(1)中所述化学改性是用表面活性剂进行改性。
8.根据权利要求1所述的方法，其特征在于，步骤(1)中所述化学改性是用聚乙二醇进行改性。
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