CN108257857A - 一种多元醇硼酸酯络合物硼扩散源及其制备方法 - Google Patents
一种多元醇硼酸酯络合物硼扩散源及其制备方法 Download PDFInfo
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- 150000005846 sugar alcohols Polymers 0.000 title claims abstract description 35
- 238000009792 diffusion process Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- ZADPBFCGQRWHPN-UHFFFAOYSA-N boronic acid Chemical compound OBO ZADPBFCGQRWHPN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 41
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000004327 boric acid Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract 2
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- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 2
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 claims description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical group COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
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- 150000002148 esters Chemical class 0.000 claims 1
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Substances BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
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- 238000001035 drying Methods 0.000 description 3
- 229910015845 BBr3 Inorganic materials 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
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- HLLSOEKIMZEGFV-UHFFFAOYSA-N 4-(dibutylsulfamoyl)benzoic acid Chemical group CCCCN(CCCC)S(=O)(=O)C1=CC=C(C(O)=O)C=C1 HLLSOEKIMZEGFV-UHFFFAOYSA-N 0.000 description 1
- 208000033999 Device damage Diseases 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 150000001638 boron Chemical class 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L21/18—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 the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- 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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- 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
- H01L21/18—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 the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- 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
- H01L21/228—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 using diffusion into or out of a solid from or into a liquid phase, e.g. alloy diffusion processes
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Abstract
本发明提出了一种适用于旋涂硼扩散制程的多元醇硼酸酯络合物硼扩散源。该硼源以多元醇和硼酸为原料,以二元醇醚为溶剂,通过多元醇和硼酸的络合作用制备多元醇硼酸酯络合物硼源。所述硼源的n(多元醇/硼酸)为0‑0.5,硼酸在溶剂中的质量百分比为1‑10wt%。将硼酸和多元醇先后加入溶剂中,在60‑90℃下搅拌0.5‑1h,停止加热后继续搅拌0.5‑1h得到澄清溶液。所得多元醇硼酸酯络合物硼源通过旋涂硼扩散制程,可在电阻率为1‑3Ω·cm的N型硅片上得到30‑150Ω/□的方块电阻,p‑n结长度为0.1‑0.5μm。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,适于大规模生产和使用。
Description
技术领域
本发明涉及晶硅太阳电池制造领域,尤其涉及用于旋涂硼扩散制程的一种多元醇硼酸酯络合物硼源及其制备方法。
背景技术
在晶硅太阳能电池制造领域,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。近几年随着n型电池的兴起,p发射极的设计和制备工艺面临新的挑战。首先,为获得高开路电压和低接触电阻,要求p-n结浅(<200nm)、掺杂浓度高(>1020cm-3);其次,为降低制造成本,要求扩散装置简易、操作简单、产量高;再者,为降低能耗和减小对器件的热损伤,要求扩散温度低(<1000oC)并减少热处理工序;还有,为实现环境友好,需使用安全无毒的硼扩散源。使用液态硼源的旋涂硼扩散制程可满足以上要求,是未来制备p发射极的主要技术之一。
目前,大部分电池产线采用BBr3气相反应硼扩散制程。扩散装置包括含有液态三溴化硼的源瓶、携带硼源并使之气化的进气系统以及扩散炉。扩散过程为先通过氮气携带三溴化硼进入扩散炉,在900℃左右将其沉积在硅片上,并在氧气作用下使之转变为氧化硼。随后在950-1000℃进行高温扩散。其缺点是气路系统复杂、工序繁重、扩散均匀性较低,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以Al2O3、SiO2以及BN成分为主,氧化物成分约占总质量的30~70%,BN成分的含有率为70~30%,氧化物中Al2O3/SiO2的摩尔比为1.0~2.4。由于复合烧结体中含有多种杂质,其纯度难以保证。此外该复合烧结体需通过热压烧结,烧结温度高(1400-1800℃),增加了制备的难度。公开号为CN103714879A的发明专利申请文件中公开了一种由硼硅纳米粒子组成的硼硅浆,可通过丝网印刷技术制备p型发射极或背场。这种方法的优点在于可减少硅片翘曲、减少碎片率,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。公开号为CN102333827A的专利申请文件中公开了一种使用非接触印刷法在半导体衬底中形成硼掺杂区域用的含硼墨和制造这种含硼墨的方法。这种含硼墨的浓度和铺展系数方便调节,且非接触的沉积方式减少了对硅片的机械损伤。但使用这种硼墨需要增加喷墨打印设备,设备成本过高,且打印精度较低,导致扩散方阻不均匀。
旋涂硼扩散工艺制程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,具备良好的流动性、铺展性和成膜性;3)硼含量高、扩散活性好。通过多元醇与硼酸的络合作用形成的多元醇硼酸酯络合物分散溶液具备这些性质。
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多元醇硼酸酯络合物硼源,它是以多元醇和硼酸为原料、以二元醇醚作为溶剂,通过多元醇和硼酸的络合作用形成硼酸酯络合物。
所述多元醇硼酸酯络合物硼源中硼酸在溶剂中的质量百分浓度为1-10wt%。
所述多元醇硼酸酯络合物中多元醇和硼酸的摩尔比为0-0.5。当摩尔比大于0.5时,所述硼源易出现浑浊现象,导致产物无法用于旋涂扩散。
所述多元醇为经过脱水的葡萄糖、甘露醇和山梨醇。
所述反应溶剂为乙二醇甲醚、乙二醇乙醚、乙二醇二甲醚、乙二醇二乙醚、二乙二醇二甲醚、二乙二醇二乙醚、乙二醇乙醚乙酸酯、丙二醇甲醚、丙二醇甲醚醋酸酯等二元醇醚类溶剂。
所述多元醇硼酸酯络合物硼源的制备方法:按设定的硼浓度和n(多元醇/硼酸)计算所需硼酸和多元醇的量并准确称量。先将硼酸倒入溶剂中,于60-90℃下加热搅拌。待硼酸溶解后,再将多元醇加入溶液中,继续加热搅拌0.5-1h。随后停止加热并继续搅拌0.5-1h。
上述制备方法的特征在于反应的温度设定在60-90℃之间。低于60℃,反应时间过长,且硼酸受溶解度限制无法完全溶解;超过90℃,溶剂快速挥发并会导致多元醇的碳化。
上述制备方法的特征在于加热反应时间设定在0.5-1h。小于0.5h,络合反应不充分,多元醇易沉淀。大于0.5h,溶剂挥发损失。
上述制备方法的另一个特征在于加热停止后需继续搅拌0.5-1h。小于0.5h,冷却时硼源易分相。
该制备方法的反应条件温和、无需任何添加剂,产物为低粘度(<100mPa·s)无色透明溶液。
所述硼源的特征在于通过多元醇与硼酸的络合作用提高了硼的稳定性和均匀性,同时硼的浓度也可自由调节。
所述多元醇硼酸酯络合物硼源的使用方法:量取1ml硼源,通过匀胶机旋涂于156×156mm2 硅片表面,并在90-150℃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℃温度下进行硼扩散制程,期间氮氧流量的比例不小于70%。
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90-150℃,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70%,氧气流量过高会导致扩散结深减小。
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。
附图说明
附图1为实施例1硼源的红外透过光谱图。
附图2为实施例2中涂敷硼源后硅片的扫描电镜图。
附图3为实施例3中扩散后硅片的载流子浓度分布图。
附图4为实施例5硼源的黏度特性曲线。
具体实施方式
实施例1
称取6.183g硼酸,量取100ml乙二醇乙醚,倒入150ml烧杯中。将烧杯置于恒温磁粒搅拌器,于80℃下搅拌0.5h。称取9.008g葡萄糖倒入烧杯中,于80℃下搅拌0.5h。停止加热并继续搅拌0.5h,将溶液收集于聚丙烯试管内。设定甩胶机转速为2500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90℃、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,扩散后将硅片浸入10%HF溶液浸泡10min。
实施例2
称取6.183g硼酸,量取100ml乙二醇乙醚,倒入150ml烧杯中。将烧杯置于恒温磁粒搅拌器,于60℃下搅拌1h。称取9.008g葡萄糖倒入烧杯中,于90℃下搅拌0.5h。停止加热并继续搅拌1h,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90℃、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,氮气/氧气流量比为90/10的气氛下扩散30min,扩散后将硅片浸入10%HF溶液浸泡10min。
实施例3
称取6.183g硼酸,量取100ml乙二醇乙醚,倒入150ml烧杯中。将烧杯置于恒温磁粒搅拌器,于60℃下搅拌1h。称取6.756g葡萄糖倒入烧杯中,于80℃下搅拌0.5h。停止加热并继续搅拌0.5h,将溶液收集于聚丙烯试管内。设定甩胶机转速为2500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90℃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85/15的气氛下扩散30分钟,扩散后将硅片浸入10%HF溶液浸泡10min。
实施例4
称取6.183g硼酸,量取100ml乙二醇乙醚,倒入150ml烧杯中。将烧杯置于恒温磁粒搅拌器,于70℃下搅拌0.5h。称取9.108g甘露醇倒入烧杯中,于80℃下搅拌0.5h。停止加热并继续搅拌0.5h,将溶液收集于聚丙烯试管内。设定甩胶机转速为2500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90℃、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,扩散后将硅片浸入10%HF溶液浸泡10min。
实施例5
称取3.092g硼酸,量取100ml丙二醇甲醚,倒入150ml烧杯中。将烧杯置于恒温磁粒搅拌器,于60℃下搅拌0.5h。称取4.504g葡萄糖倒入烧杯中,于80℃下搅拌0.5h。停止加热并继续搅拌0.5h,将溶液收集于聚丙烯试管内。设定甩胶机转速为2500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90℃、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,扩散后将硅片浸入10%HF溶液浸泡10min。
Claims (9)
1.一种多元醇硼酸酯络合物硼扩散源及其制备方法,其特征在于硼源由多元醇和硼酸形成的络合物以及二元醇醚类溶剂组成,其制备方法是:按设定的硼浓度和n(多元醇/硼酸)称取硼酸、多元醇和溶剂,先将硼酸倒入溶剂中加热搅拌,待其溶解后再将多元醇加入溶液中继续加热搅拌,随后停止加热并继续搅拌至室温。
2.根据权利要求1所述的硼源的制备方法,其特征在于所述多元醇为脱水的葡萄糖、甘露醇和山梨醇。
3.根据权利要求1和2所述的液态硼源的制备方法,其特征在于多元醇和硼酸的摩尔比为0-0.5。
4.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乙二醇甲醚、乙二醇乙醚、乙二醇二甲醚、乙二醇二乙醚、二乙二醇二甲醚、二乙二醇二乙醚、乙二醇乙醚乙酸酯、丙二醇甲醚、丙二醇甲醚醋酸酯等二元醇醚类溶剂。
5.根据权利要求1和4所述的液态硼源的制备方法,其特征在于硼酸在溶剂中的质量百分浓度为1-10wt%。
6.根据权利要求1所述的液态硼源的制备方法,其特征在于加热搅拌的温度为60-90℃。
7.权利要求1和所述的液态硼源及的制备方法,其特征在于反应加料顺序为先硼酸后多元醇。
8.根据权利要求1和7所述的液态硼源的制备方法,其特征在于加入多元醇后的加热搅拌时间为0.5-1h。
9.根据权利要求1所述的液态硼源的制备方法,其特征在于停止加热后需继续搅拌0.5-1h至室温。
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CN113410134A (zh) * | 2021-06-08 | 2021-09-17 | 河南大学 | 一种实现低温扩散的硼源 |
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