CN115148848A - 链式吸杂用磷源及其制备方法和应用 - Google Patents
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 81
- 239000011574 phosphorus Substances 0.000 title claims abstract description 81
- 239000012535 impurity Substances 0.000 title claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000009792 diffusion process Methods 0.000 claims abstract description 44
- 239000003960 organic solvent Substances 0.000 claims abstract description 39
- 238000005247 gettering Methods 0.000 claims abstract description 37
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 229910019142 PO4 Inorganic materials 0.000 claims description 13
- 239000010452 phosphate Substances 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 5
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 5
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 4
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 235000011180 diphosphates Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 125000005456 glyceride group Chemical group 0.000 claims description 3
- TVZISJTYELEYPI-UHFFFAOYSA-N hypodiphosphoric acid Chemical compound OP(O)(=O)P(O)(O)=O TVZISJTYELEYPI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- -1 phosphate ester Chemical class 0.000 claims description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005696 Diammonium phosphate Substances 0.000 claims description 2
- 239000006012 monoammonium phosphate Substances 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 abstract description 9
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical group OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229940005657 pyrophosphoric acid Drugs 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 description 2
- 125000004437 phosphorous atom Chemical group 0.000 description 2
- 229940048084 pyrophosphate Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 1
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 1
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
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- H01L21/22—Diffusion of impurity materials, e.g. doping materials, electrode materials, into or out of a semiconductor body, or between semiconductor regions; Interactions between two or more impurities; Redistribution of impurities
- H01L21/2225—Diffusion sources
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Abstract
本发明公开了一种链式吸杂用磷源，其各组分的质量百分含量为：磷源前驱体2%～10%，聚乙二醇1%～20%，柠檬酸1%～5%，有机溶剂1%～10%，余量为水。本发明还提供上述链式吸杂用磷源的制备方法和应用。本发明的磷源能很好的匹配现有链式扩散吸杂设备，可避免或改善现有磷源链式高温扩散吸杂产生偏磷酸、焦磷酸残留的问题。本发明通过调整磷源配方，优化链式扩磷吸杂的温度、时间、氛围等参数，使扩磷的扩散均匀性、结深等性质较常规磷酸混合液有所提升。采用本发明制备的磷源，结合链式设备进行快速磷扩散，可在较短的时间内达到与传统管式扩散一样的扩散水平，使链式扩散的工业化应用得以实现，解决了目前管式扩散设备及自动化昂贵的问题。
Description
技术领域
本发明涉及光伏领域，具体涉及一种链式吸杂用磷源及其制备方法和应用。
背景技术
晶体硅中杂质的P吸除是一种众所周知的常规方法，通过P捕获杂质来延长整体少数载流子的寿命从而改善电池性能。重掺P杂质层可提供大量吸杂机制：分凝机制、应力吸杂机制等。目前常规PERC和TOPCon电池制备过程中，就是利用磷扩散制备的pn结良好的吸杂效果。
在太阳能电池领域，磷扩散主要以POCl3为前驱体管式高温扩散为主，扩散设备及自动化昂贵，前驱体POCl3剧毒且有强腐蚀性。在应用于吸杂过程中，为实现更好的双面吸杂效果，产能损失较大，且随着薄片化需求的不断发展，管式吸杂高碎片风险的问题逐渐突出，因而链式吸杂应运而生。
链式吸杂与链式扩散类似，目前研究的磷源主要以简单的磷酸混合溶液以及Filmtronics、Honeywell等公司研发的进口磷源为主。单纯的磷酸混合溶液，在高温过程中不可避免的会生成难以去除的偏磷酸、焦磷酸等物质，扩散不均匀，表面死层较厚，制备的PN结质量较差，结深较浅，使吸杂性能无法提高，且为获得Filmtronics、Honeywell等公司研发的磷源价格十分昂贵，制约了其工业化的研究与应用。
有鉴于此，制备一种价格低廉的适用于链式吸杂的磷源，使其在链式设备上应用能达到优于管式吸杂的水平至关重要。
发明内容
为了解决现有技术的缺陷，本发明提供一种链式吸杂用磷源，其各组分的质量百分含量为：磷源前驱体2%～10%，聚乙二醇1%～20%，柠檬酸1%～5%，有机溶剂1%～10%，余量为水。
优选的，所述磷源前驱体选自磷酸、P2O5、磷酸二氢铵、磷酸氢二铵、多聚磷酸、磷酸酯中的一种或几种。
优选的，所述磷酸酯选自焦磷酸酯、聚磷酸酯、磷酸多酯、亚磷酸酯、连二磷酸酯、磷酸三乙酯、2-乙基己基磷酸酯、次磷酸酯中的一种或几种。
优选的，所述有机溶剂选自酯类有机溶剂、醇类有机溶剂、酰胺类有机溶剂中的一种或几种。
优选的，所述酯类有机溶剂选自甲酸酯类有机溶剂、乙酸酯类有机溶剂、甘油酯类有机溶剂、磷酸酯类有机溶剂、磷酯类有机溶剂、硅酸酯类有机溶剂中的一种或几种。
优选的，所述醇类有机溶剂选自甲醇、乙醇、异丙醇中的一种或几种。
本发明还提供上述链式吸杂用磷源的制备方法，包括如下步骤：将质量百分含量为2%～10%的磷源前驱体、1%～20%的聚乙二醇、1%～5%的柠檬酸、1%～10%有机溶剂以及余量的水投入反应器中，于25～150℃反应2～48h，过滤得到磷源。
本发明还提供一种链式吸杂方法，在链式扩散设备中对表面沉积上述磷源的硅片进行扩磷吸杂（磷源扩散和磷吸杂）。
优选的，采用旋涂、喷涂或滚涂方式沉积磷源。
优选的，磷源的沉积厚度为1～2μm；扩磷吸杂的工艺条件：温度为200～900℃，时间为10～200s，氛围为氮气或者氧气。
本发明的优点和有益效果在于：
本发明的磷源能很好的匹配现有的链式扩散吸杂设备，本发明的磷源可避免或改善现有磷源（磷酸混合液）链式高温扩散吸杂产生偏磷酸、焦磷酸残留的问题。
现有磷源主要成分为磷酸，磷酸在200℃左右脱水形成焦磷酸，在300℃形成偏磷酸，继续升温，偏磷酸脱水形成五氧化二磷起到扩散的效果。现有以磷酸为主要成分的磷源(主要应用与链式扩散领域)，为获得较好的扩散或吸杂效果，需要较高浓度的磷酸，10%以上，在高温过程中磷酸脱水，形成大量的偏磷酸固体，在炉口聚集，较难通过简单的清洗手段去除，影响设备外观及使用。
本发明摈弃传统的磷酸为主要成分的磷源，以P2O5、磷酸二氢铵、磷酸氢二铵、多聚磷酸、磷酸酯等混合形成复合磷源，极大的减少溶液中磷酸的含量，减轻偏磷酸、焦磷酸等物质的残留，对改善炉口偏磷酸固体沉淀问题改善明显。
本发明通过调整磷源配方，优化链式扩磷吸杂的温度、时间、氛围等参数，使扩磷的扩散均匀性、结深等性质较常规磷酸混合液有所提升，且能达到与管式扩散一致的水平。
磷源中添加柠檬酸组分，可以减轻活性组分与载体之间的相互作用，进而改善活性磷原子在硅片表面的分散状态，使磷在硅片表面分散更加均匀，获得更好的扩散均匀性。
采用复合磷源，磷源中增加磷酸二氢铵、磷酸氢二铵等组分，溶液中的产生的大量铵根离子，扩散过程中在硅片体内形成大量空穴，空穴辅助磷源扩散，使活性磷原子获得更深的扩散深度。
本发明的磷源低毒，且原料易获得，价格低廉。
采用本发明制备的磷源，结合链式设备进行快速磷扩散，可在较短的时间内达到与传统管式扩散一样的扩散水平，使链式扩散的工业化应用得以实现，解决了目前管式扩散设备及自动化昂贵的问题。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
本发明提供一种链式吸杂方法，包括如下步骤：
1）制备链式吸杂用磷源：将质量百分含量为2%～10%的磷源前驱体、1%～20%的聚乙二醇、1%～5%的柠檬酸、1%～10%有机溶剂以及余量的水投入反应器中，于25～150℃反应2～48h，过滤得到磷源；其中：
所述磷源前驱体选自磷酸、P2O5、磷酸二氢铵、磷酸氢二铵、多聚磷酸、磷酸酯中的一种或几种；
具体的，所述磷酸酯选自焦磷酸酯、聚磷酸酯、磷酸多酯、亚磷酸酯、连二磷酸酯、磷酸三乙酯、2-乙基己基磷酸酯、次磷酸酯中的一种或几种；
所述有机溶剂选自酯类有机溶剂、醇类有机溶剂、酰胺类有机溶剂中的一种或几种；
具体的，所述酯类有机溶剂选自甲酸酯类有机溶剂、乙酸酯类有机溶剂、甘油酯类有机溶剂、磷酸酯类有机溶剂、磷酯类有机溶剂、硅酸酯类有机溶剂中的一种或几种；
具体的，所述醇类有机溶剂选自甲醇、乙醇、异丙醇中的一种或几种；
2）在链式扩散设备中对表面沉积上述磷源的硅片进行扩磷吸杂（即磷源扩散和磷吸杂）；具体的：
采用旋涂、喷涂或滚涂方式在硅片表面沉积磷源，磷源的沉积厚度为1～2μm；
链式扩散设备中扩磷吸杂的工艺条件：温度为200～900℃，时间为10～200s，氛围为氮气或者氧气。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.链式吸杂用磷源，其特征在于，其各组分的质量百分含量为：磷源前驱体2%～10%，聚乙二醇1%～20%，柠檬酸1%～5%，有机溶剂1%～10%，余量为水。
2.根据权利要求1所述的链式吸杂用磷源，其特征在于，所述磷源前驱体选自磷酸、P2O5、磷酸二氢铵、磷酸氢二铵、多聚磷酸、磷酸酯中的一种或几种。
3.根据权利要求2所述的链式吸杂用磷源，其特征在于，所述磷酸酯选自焦磷酸酯、聚磷酸酯、磷酸多酯、亚磷酸酯、连二磷酸酯、磷酸三乙酯、2-乙基己基磷酸酯、次磷酸酯中的一种或几种。
4.根据权利要求1所述的链式吸杂用磷源，其特征在于，所述有机溶剂选自酯类有机溶剂、醇类有机溶剂、酰胺类有机溶剂中的一种或几种。
5.根据权利要求4所述的链式吸杂用磷源，其特征在于，所述酯类有机溶剂选自甲酸酯类有机溶剂、乙酸酯类有机溶剂、甘油酯类有机溶剂、磷酸酯类有机溶剂、磷酯类有机溶剂、硅酸酯类有机溶剂中的一种或几种。
6.根据权利要求4所述的链式吸杂用磷源，其特征在于，所述醇类有机溶剂选自甲醇、乙醇、异丙醇中的一种或几种。
7.权利要求1至6中任一项所述的链式吸杂用磷源的制备方法，其特征在于，包括如下步骤：将质量百分含量为2%～10%的磷源前驱体、1%～20%的聚乙二醇、1%～5%的柠檬酸、1%～10%有机溶剂以及余量的水投入反应器中，于25～150℃反应2～48h，过滤得到磷源。
8.链式吸杂方法，其特征在于，在链式设备中对表面沉积磷源的硅片进行扩磷吸杂，且磷源采用权利要求1至7中任一项所述的磷源。
9.权利要求8所述的链式吸杂方法，其特征在于，采用旋涂、喷涂或滚涂方式沉积磷源。
10.权利要求8所述的链式吸杂方法，其特征在于，磷源的沉积厚度为1～2μm；扩磷吸杂的工艺条件：温度为200～900℃，时间为10～200s，氛围为氮气或者氧气。
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