CN107195543A - 一种晶硅太阳能电池用液态硼源及其制备方法 - Google Patents
一种晶硅太阳能电池用液态硼源及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 35
- 229910052710 silicon Inorganic materials 0.000 title abstract description 35
- 239000010703 silicon Substances 0.000 title abstract description 35
- 239000013078 crystal Substances 0.000 title description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
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Abstract
本发明提出了一种适用于旋涂硼扩散制程的聚硼硅氧烷硼源。该硼源以硅烷和硼酸为原料，采用溶胶凝胶法制备，采用的硼源的n(B/Si)＝m，其中：0＜m≤0.6。采用的硅烷的化学式为(R1)xSi(OR2)y，其中：R1为‑CH3或‑CH2CH3，R3为‑CH3、‑CH2CH3或‑CH(CH3)2，x＝1或2，y＝3或2，且x+y＝4。将硅烷和硼酸的混合溶液在20‑60℃下搅拌1‑3天直至溶液由浑浊变为澄清，所得聚硼硅氧烷液态硼源通过旋涂、烘干和扩散等工艺，可在N型硅片上得到30‑200Ω/□的方块电阻。该硼源的浓度和纯度高，适用于旋涂硼扩散制程。其制备方法简单易行、合成条件温和、材料成本低，适于大规模生产和利用。
Description
技术领域
本发明涉及晶硅太阳电池制造领域，尤其涉及用于硼扩散制程的一种新型硼源及其制备方法。
背景技术
在硅基半导体器件制造领域，硼扩散是重要的p型掺杂技术，可用于在n型硅基体上制备p-n结器件。近年来兴起的n型晶硅太阳电池对制备p发射极的硼扩散技术提出了特定要求。首先，为获得高的光电转换效率，要求浅结(<200nm)、重掺杂(>1020cm-3)；再者，为减小对器件的热损伤，要求扩散温度低(<1000℃)；还有，为降低制造成本和环境友好，要求扩散装置和操作简单、以及使用安全无毒的硼源。使用液态硼源的旋涂硼扩散制程可满足以上要求，因而被制造业界认为是未来制备p发射极的主要技术。
目前，大部分电池产线采用BBr3气相反应硼扩散制程，公开号为CN103633190A的发明专利申请文件中公开了一种晶体硅太阳能电池硼扩散的装置及方法。该装置由炉管、硼源瓶以及尾气瓶组成。硼源瓶中的液态硼源先经载气(氮气)进行气化后通过炉管壁上的进气口送入扩散炉内，紧接着在氮气和氧气的调节下进行沉积。其缺点是气路系统复杂、工序繁重并且BBr3有较强的腐蚀性和毒性。有少数电池产线采用BN片与硅片叠层的方式进行硼扩散制程，公开号为CN101542687的发明专利申请文件中公开了一种复合烧结体硼扩散源。其中所述复合烧结体含有Al2O3、SiO2以及BN成分，Al2O3和SiO2成分的合计含有率为30～70质量％，BN成分的含有率为30～70质量％，并且Al2O3/SiO2的摩尔比为1.0～2.4。其缺点是复合烧结体需通过热压烧结，烧结温度高(1400-1800℃)，制备复杂。且复合烧结体硼源中杂质较多，纯度难以保证。文献[J.Mater.Sci.Technol.,2013,29(7):652-654]报道了一种由硼硅纳米粒子组成的硼浆，以及通过丝网印刷的方式将硼浆印制在硅片表面进行硼扩散制程。这种方法的缺点在于需要添置专门的丝网印刷设备、硼浆的制备也较为复杂。文献[J.Phys.Chem.Lett.,2013,4(21):3741–3746]报道了一种有机硼聚合物(聚乙烯基硼酸频哪醇酯-PVBAPE)，并利用匀胶机将PVBAPE旋涂在硅片表面进行硼扩散制程。这种旋涂硼扩散技术的特点是操作简单、设备成本低、扩散质量好、生产效率高，但PVBAPE合成复杂、价格昂贵、硼含量低，不符合工业化生产的要求。
旋涂硼扩散技术的工业化应用要求所采用的硼源需具备以下基本性质：1)结构简单、安全无毒、易于大量合成、成本低；2)呈液态或可均匀分散于溶剂中，旋涂成膜性好；3)硼含量高、扩散活性好。具有B-O-Si网络结构的聚硼硅氧烷可具备这些性质。
发明内容
为解决上述问题，本发明提出了一种适用于旋涂硼扩散制程的聚硼硅氧烷液态硼源，它是以硅烷和硼酸为原料，采用溶胶凝胶法制备,其结构如下：
其中R1为-CH3或-CH2CH3，R2为-OH、-CH3或-CH2CH3。
所述聚硼硅氧烷硼源的n(B/Si)＝m，其中：0＜m≤0.6，m越大，硼的浓度越高。当m大于0.6时，所述硼源易出现浑浊现象，导致产物无法用于旋涂扩散。
所用硅烷的化学式为(R1)xSi(OR3)y。其中，R1为-CH3或-CH2CH3，R3为-CH3、-CH2CH3或-CH(CH3)2，x＝1或2，y＝2或3，且x+y＝4。可以是一种硅烷或以上。
所述聚硼硅氧烷的制备方法：按设定的硼硅比和产物的量，计算所需原料硅烷和硼酸的量，并准确称量；将原料直接混合，在20-60℃下搅拌1-3天。
上述制备方法的特征在于搅拌反应的温度设定在20-60℃之间。低于20℃，反应时间过长；超过60℃，反应生成的甲醇、乙醇以及异丙醇等小分子会快速挥发，造成硼的大量损失。上述制备方法的另一个特征在于反应时间根据反应温度设定在1-3天，温度越高时间越短。小于1天，溶胶凝胶反应不充分，体系中含有大量未溶解的硼酸；超过3天，体系中的硅烷会发生自缩聚，导致黏度增大。
该制备方法的反应条件温和、无需任何添加剂。产物为液态聚硼硅氧烷，它可直接作为硼源使用，也可分散在各种醇、醚或醇醚类溶剂中加以使用。
所述聚硼硅氧烷的特征在于具有B-O-Si网络结构，提高了B的稳定性和均匀性，同时硼的浓度也可自由调节。
所述聚硼氧硅烷作为硼源的使用方法：将液态聚硼硅氧烷或其分散在醇、醚或醇醚类溶剂的混合溶液通过匀胶机旋涂硅片表面，并在90-200℃温度下加热1-2min烘干；将烘干后的硅片放入扩散炉内，于900-1000℃温度下进行扩散制程，期间氮氧流量的比例不小于90％。
所述硼源应用方法的特征在于可直接采用传统的旋涂和扩散工艺。所述烘干温度为90-200℃，温度过低或过高都不利于硼源的均匀固化。
所述扩散气氛为氮氧流量比例不小于90％，氧气流量过高不利于硼的分解。
上述硼源的制备方法简单易行，反应条件温和；硼源组分可自由调节。硼源不含水，不会造成硼的水解；硼源原料易得，制备成本低，适合大规模的生产。
具体实施方式
实施例1
称取硼酸1.5208g，量取甲基三乙氧基硅烷10ml，放入50ml烧杯中。将烧杯置于恒温磁粒搅拌器，于25℃下搅拌3天，将溶液收集于聚丙烯试管内。设定甩胶机转速为2000转/分，时间为20秒，在156×156mm2硅片上滴1ml溶液进行旋涂。将旋涂后的硅片置于电加热台上并分别在60℃、120℃和150℃下各加热30秒。随后将硅片插入石英舟，并推入950℃的管式炉内，在纯氮气气氛下扩散30分钟，扩散后取出硅片即可。
实施例2
称取硼酸1.7163g，量取二甲基二乙氧基硅烷10ml，放入50ml烧杯中。将烧杯置于恒温磁粒搅拌器，于25℃下搅拌3天，将溶液收集于聚丙烯试管内。设定甩胶机转速为2000转/分，时间为20秒，在156×156mm2硅片上滴1ml溶液进行旋涂。将旋涂后的硅片置于电加热台上并分别在60℃、120℃和150℃下各加热30秒。随后将硅片插入石英舟，并推入950℃的管式炉内，在纯氮气气氛下扩散30分钟，扩散后取出硅片即可。
实施例3
称取硼酸1.54575g，分别量取1.27ml甲基三乙氧基硅烷和7.88ml二甲基二乙氧基硅烷，放入50ml烧杯中。将烧杯置于恒温磁粒搅拌器，于25℃下搅拌3天，将溶液收集于聚丙烯试管内。设定甩胶机转速为2000转/分，时间为20秒，在156×156mm2硅片上滴1ml溶液进行旋涂。将旋涂后的硅片置于电加热台上并分别在60℃、120℃和150℃下各加热30秒。随后将硅片插入石英舟，并推入950℃的管式炉内，在纯氮气气氛下扩散30分钟，扩散后取出硅片即可。
实施例4
称取硼酸1.54575g，分别量取1.27ml甲基三乙氧基硅烷和7.88ml二甲基二乙氧基硅烷，放入50ml烧杯中。将烧杯置于恒温磁粒搅拌器，于50℃下搅拌1天，将溶液收集于单口烧瓶内。将烧瓶抽真空并于90℃下进行旋转蒸馏，蒸馏后收集烧瓶内的产物并将其溶于乙二醇甲醚中待用。设定甩胶机转速为2500转/分，时间为30秒，在156×156mm2硅片上滴1ml溶液进行旋涂。将旋涂后的硅片置于电加热台上并分别在60℃、120℃和150℃下各加热30秒。随后将硅片插入石英舟，并推入950℃的管式炉内，在纯氮气气氛下扩散30分钟，扩散后取出硅片即可。
实施例5
称取硼酸1.54575g，分别量取1.27ml甲基三乙氧基硅烷和7.88ml二甲基二乙氧基硅烷，放入50ml烧杯中。将烧杯置于恒温磁粒搅拌器，于40℃下搅拌2天，将溶液收集于聚丙烯试管内。设定甩胶机转速为2000转/分，时间为20秒，在156×156mm2硅片上滴1ml溶液进行旋涂。将旋涂后的硅片置于电加热台上并分别在60℃、120℃和150℃下各加热30秒。随后将硅片插入石英舟，并推入970℃的管式炉内，在氮气/氧气流量比为90/10的气氛下扩散40分钟，扩散后取出硅片即可。
附图说明
图1为实施例1硼源和实例2硼源的热重曲线。
图2为实施例1硼源的红外透过光谱图。
图3为实施例3中涂敷硼源后硅片的扫描电镜图。
图4为实施例2中扩散后硅片的载流子浓度分布图。
Claims (6)
1.一种液态硼源及其制备方法，其特征在于液态硼源由聚硼硅氧烷和溶剂组成，聚硼硅氧烷的结构如下:
其中R1为-CH3或-CH2CH3，R2为-OH、-CH3或-CH2CH3。其制备方法是：按一定摩尔比例称取、混合有机硅烷和硼酸，将混合物在20-60℃搅拌1-3天。
2.根据权利要求1所述的液态硼源的制备方法，其特征在于硼源的0＜n(B/Si)≤0.6。
3.根据权利要求1所述的液态硼源的制备方法，其特征在于有机硅烷的化学式为(R1)xSi(OR3)y，其中：R1为-CH3或-CH2CH3，R3为-CH3、-CH2CH3或-CH(CH3)2，x＝1或2，y＝2或3，且x+y＝4。
4.根据权利要求1和3所述的液态硼源制备方法，其特征在于所述的有机硅烷可以是一种及以上。
5.根据权利要求1所述的液态硼源的制备方法，其特征在于所述溶剂为醇类、醚类或醇醚类中的一种或者它们的混合。
6.权利要求1和5所述的液态硼源及其制备方法，其特征在于聚硼硅氧烷和溶剂的体积比为1:1。
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| CN108110090B (zh) * | 2018-01-11 | 2020-03-06 | 江苏顺风光电科技有限公司 | 一种n型双面电池制备方法 |
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