CN115274893B - 一种稀土掺杂硅基薄膜材料及其制备方法 - Google Patents
一种稀土掺杂硅基薄膜材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 95
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 63
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 34
- 239000010703 silicon Substances 0.000 title claims abstract description 34
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 20
- 239000010408 film Substances 0.000 claims description 27
- 238000004544 sputter deposition Methods 0.000 claims description 25
- -1 rare earth ions Chemical class 0.000 claims description 22
- 238000000137 annealing Methods 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 16
- 239000010409 thin film Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002210 silicon-based material Substances 0.000 claims description 10
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005468 ion implantation Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 6
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 238000002513 implantation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 239000012300 argon atmosphere Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- QNWMNMIVDYETIG-UHFFFAOYSA-N gallium(ii) selenide Chemical compound [Se]=[Ga] QNWMNMIVDYETIG-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种稀土掺杂硅基薄膜材料及其制备方法，属于光伏材料制备技术领域。所述稀土掺杂硅基薄膜材料的制备包括多晶材料的制备、磁控溅射处理、稀土元素的掺杂三个主要步骤。本发明提供的制备工艺简单，可控性强；制备得到的稀土掺杂硅基薄膜材料光电转化率高，具有良好的应用前景。
Description
技术领域
本发明属于光伏材料制备技术领域，具体涉及一种稀土掺杂硅基薄膜材料及其制备方法。
背景技术
随着不可再生能源的消费，加强风能、太阳能、潮汐能等可再生能源的开发利用十分重要。其中，太阳能利用过程中最重要的是太阳能电池，其是通过光电效应或者光化学效应直接把光能转化为电能的装置；根据材料的不同，太阳能电池可以分为硅太阳能电池、多元化合物薄膜太阳能电池、聚合物多层修饰电极型电池、有机太阳能电池、纳米晶太阳能电池、塑料太阳能电池等。其中，根据硅材料的不同，硅太阳能电池又可分为单晶硅、多晶硅、非晶硅等。当前，太阳能电池的发展已经经历了三代，第一代为单晶硅太阳能电池，第二代为多晶硅、非晶硅等太阳能电池，第三代就是铜铟镓硒CIGS(CIS中掺入Ga)等化合物薄膜太阳能电池以及薄膜Si系太阳能电池。
现有技术中，专利文献CN106340552B公开了一种稀土掺杂的光伏薄膜材料，其制备方法如下：步骤1，将铜盐放入至反应釜中，加入溶剂与催化剂，搅拌均匀得到铜液；步骤2，将硫化物缓慢加入至无水乙醇中，搅拌均匀，加入稳定剂，得到硫液；步骤3，将硫液缓慢滴加至铜液中，搅拌均匀，得到混合液，密封静置2-5h；步骤4，将EDTA缓慢滴加至缓和液，并形成曝气反应3-5h，得到络合液；步骤5，将氧化钇加入至络合液中，搅拌均匀，然后进行水浴超声反应2-4h；步骤6，将超声反应后的络合液中加入引发剂，进行回流曝气还原反应3-5h；步骤7，将还原反应后的还原液加入分散剂，并进行恒温蒸馏反应，即可得到光伏薄膜材料。整个制备工艺相对复杂，使用到的硫化氢毒性高，且光电转化效率还有待进一步提高。
发明内容
针对现有技术存在的不足，本发明的目的之一在于提供一种稀土掺杂硅基薄膜材料，光电转化效率高，应用前景好。
本发明的另外一个目的在于提供上述稀土掺杂硅基薄膜材料的制备方法，制备工艺简单，可操作性强。
为了实现上述目的，本发明采用如下技术方案：
一种稀土掺杂硅基薄膜材料，包括如下步骤：
S1、多晶材料的制备：将ZnO与Ga2O3混合研磨后进行压片，随后进行煅烧；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到硅基材料上，得材料a；
S3、稀土元素的掺杂：在惰性气氛中，将步骤S2所得材料a先进行第一次退火处理，得材料b，随后注入稀土离子；最后，在惰性气氛中，进行第二次退火处理，即得稀土掺杂硅基薄膜材料；
其中，稀土离子由摩尔比为1～3：1～3：1的Gd2O3、La2O3、Sc2O3均匀混合而成。
优选的，步骤S1中，ZnO与Ga2O3的摩尔比为1.2～1.8：1。
优选的，步骤S1中，压片压力为6～10MPa，保压时间为3～8min；煅烧温度为1100～1500℃，煅烧时间为6～24h。
优选的，步骤S2中，所述硅基材料选自单晶硅光伏薄膜材料、多晶硅光伏薄膜材料中的一种或两种。
优选的，步骤S2中，磁控溅射的工艺条件为：真空压力为6×10-3～9×10-3Pa，氦气流量为35～45sccm，溅射压强为3～10Pa，基片温度为380～500℃，射频电源溅射功率为90～110W，溅射时间为3～6h。
优选的，步骤S2中，多晶材料的用量为0.15～0.55mol，硅基材料的规格为15mm×15mm×(70～85)nm。
优选的，步骤S3中，第一次退火的温度为300～700℃，退火时间为12～18min；第二次退火的温度为1050～1200℃，退火时间为22～28min。
优选的，步骤S3中，稀土离子采用离子注入法注入，真空压力为3×10-3～4×10- 3Pa，注入稀土氧化物携带的能量为120～180Kev。
优选的，步骤S3中，稀土离子的注入总剂量为1014～1018ions/cm2。
同时，本发明还要求保护由上述方法制备得到的稀土掺杂硅基薄膜材料。
与现有技术相比，本发明具有如下有益效果：
(1)本发明制备得到的稀土掺杂硅基薄膜材料具有优良的光电转化率，达到30％左右，性能十分优良。
(2)首先，本发明选用常见的ZnO和Ga2O3混合得到多晶材料；其中ZnO是良好的半导体材料，在光照激发下，能吸收能量使得原子跃迁以实现光能转化为热能，Ga2O3则能提高光电转化效率；随后，利用磁控溅射将多晶材料溅射到硅基材料表面，并随后注入稀土离子，进一步提高光电转化效率；需要特别强调的是，本发明中对于稀土离子种类的选择做了反复优化，最终注入Gd、La、Sc三种元素混合得到的稀土元素，能够使得光电转化效率最大化。
(3)本发明稀土掺杂硅基薄膜材料制备工艺简单，可控性强，具有较好的应用前景。
具体实施方式
同时，需要说明的是，本发明中的磁控溅射仪型号为JGP-450型；所用硅基材料及其他试剂或化学药品均通过市场途径购买得到。
实施例1
一种稀土掺杂硅基薄膜材料，包括如下步骤：
S1、多晶材料的制备：将摩尔比为1.4：1的ZnO与Ga2O3混合研磨后于6.5MPa下压片6min，随后于1150℃下煅烧8h；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到规格为15mm×15mm×75nm的单晶硅光伏薄膜材料上，得材料a；其中，多晶材料的用量为0.35mol；磁控溅射的工艺条件为：真空压力为7×10-3Pa，氦气流量为35sccm，溅射压强为8Pa，基片温度为420℃，射频电源溅射功率为95W，溅射时间为3.5h；
S3、稀土元素的掺杂：在氩气惰性气氛中，将步骤S2所得材料a先于650℃下退火处理14min，得材料b，随后注入总剂量为3×1015ions/cm2的含稀土离子的氧化物；最后，在氩气惰性气氛中，于1050℃下退火处理24min，即得稀土掺杂硅基薄膜材料；
其中，含稀土离子的氧化物由摩尔比为1.5：1.5：1的Gd2O3、La2O3、Sc2O3均匀混合而成。
其中，步骤S3中，稀土离子采用离子注入法注入，真空压力为3×10-3Pa，注入稀土氧化物携带的能量为140Kev。
实施例2
一种稀土掺杂硅基薄膜材料，包括如下步骤：
S1、多晶材料的制备：将摩尔比为1.6：1的ZnO与Ga2O3混合研磨后于7MPa下压片5min，随后于1200℃下煅烧7h；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到规格为15mm×15mm×75nm的单晶硅光伏薄膜材料上，得材料a；其中，多晶材料的用量为0.4mol；磁控溅射的工艺条件为：真空压力为6×10-3Pa，氦气流量为38sccm，溅射压强为7Pa，基片温度为440℃，射频电源溅射功率为100W，溅射时间为4h；
S3、稀土元素的掺杂：在氩气惰性气氛中，将步骤S2所得材料a先于670℃下退火处理12min，得材料b，随后注入总剂量为6×1015ions/cm2的含稀土离子的氧化物；最后，在氩气惰性气氛中，于1100℃下退火处理26min，即得稀土掺杂硅基薄膜材料；
其中，含稀土离子的氧化物由摩尔比为1.4：1.6：1的Gd2O3、La2O3、Sc2O3均匀混合而成。
其中，步骤S3中，稀土离子采用离子注入法注入，真空压力为4×10-3Pa，注入稀土氧化物携带的能量为130Kev。
实施例3
一种稀土掺杂硅基薄膜材料，包括如下步骤：
S1、多晶材料的制备：将摩尔比为1.5：1的ZnO与Ga2O3混合研磨后于8MPa下压片4min，随后于1200℃下煅烧6h；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到规格为15mm×15mm×75nm的单晶硅光伏薄膜材料上，得材料a；其中，多晶材料的用量为0.38mol；磁控溅射的工艺条件为：真空压力为7×10-3Pa，氦气流量为40sccm，溅射压强为9Pa，基片温度为460℃，射频电源溅射功率为110W，溅射时间为4.5h；
S3、稀土元素的掺杂：在氩气惰性气氛中，将步骤S2所得材料a先于680℃下退火处理16min，得材料b，随后注入总剂量为1×1016ions/cm2的含稀土离子的氧化物；最后，在氩气惰性气氛中，于1150℃下退火处理22min，即得稀土掺杂硅基薄膜材料；
其中，含稀土离子的氧化物由摩尔比为1.6：1.4：1的Gd2O3、La2O3、Sc2O3均匀混合而成。
其中，步骤S3中，稀土离子采用离子注入法注入，真空压力为3×10-3Pa，注入稀土氧化物携带的能量为150Kev。
对比例1
一种稀土掺杂硅基薄膜材料，包括如下步骤：
S1、多晶材料的制备：将摩尔比为1.4：1的ZnO与Ga2O3混合研磨后于6.5MPa下压片6min，随后于1150℃下煅烧8h；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到规格为15mm×15mm×75nm的单晶硅光伏薄膜材料上，得材料a；其中，多晶材料的用量为0.35mol；磁控溅射的工艺条件为：真空压力为7×10-3Pa，氦气流量为35sccm，溅射压强为8Pa，基片温度为420℃，射频电源溅射功率为95W，溅射时间为3.5h；
S3、稀土元素的掺杂：在氩气惰性气氛中，将步骤S2所得材料a先于650℃下退火处理14min，得材料b，随后注入总剂量为3×1015ions/cm2的含稀土离子的氧化物；最后，在氩气惰性气氛中，于1050℃下退火处理24min，即得稀土掺杂硅基薄膜材料；
其中，含稀土离子的氧化物为Sc2O3。
其中，步骤S3中，稀土离子采用离子注入法注入，真空压力为3×10-3Pa，注入稀土氧化物携带的能量为140Kev。
将实施例1～3和对比例1制备得到的稀土掺杂硅基薄膜材料进行光电转化率的测试，具体测试方法为：测试各稀土掺杂硅基薄膜材料单位面积输出最大功率与单位面积入射光能量，并基于下述公式进行计算光电转化率。
光电转化率(％)＝单位面积输出最大功率/单位面积入射光能量*100。
测试结果见表1所示。
| 光电转化率/％ | |
| 实施例1 | 30.2 |
| 实施例2 | 30.8 |
| 实施例3 | 31.1 |
| 对比例1 | 27.9 |
从表1中可以看到，本申请各实施例制备得到的稀土掺杂硅基薄膜材料的光电转化率均高于30％，性能佳，具有良好的应用前景。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (6)
1.一种稀土掺杂硅基薄膜材料，其特征在于，包括如下步骤：
S1、多晶材料的制备：将ZnO与Ga2O3混合研磨后进行压片，随后进行煅烧；煅烧完成后即得多晶材料；
S2、磁控溅射处理：将步骤S1制备得到的多晶材料通过磁控溅射的方式溅射到硅基材料上，得材料a；
S3、稀土元素的掺杂：在惰性气氛中，将步骤S2所得材料a先进行第一次退火处理，得材料b，随后注入稀土离子；最后，在惰性气氛中，进行第二次退火处理，即得稀土掺杂硅基薄膜材料；
其中，稀土离子由摩尔比为1~3：1~3：1的Gd2O3、La2O3、Sc2O3均匀混合而成；
其中，步骤S1中，ZnO与Ga2O3的摩尔比为1.2~1.8：1；
其中，步骤S1中，压片压力为6~10MPa，保压时间为3~8min；煅烧温度为1100~1500℃，煅烧时间为6~24h；
其中，步骤S2中，磁控溅射的工艺条件为：真空压力为6×10-3~9×10-3Pa，氦气流量为35~45sccm，溅射压强为3~10Pa，硅基材料的温度为380~500℃，射频电源溅射功率为90~110W，溅射时间为3~6h。
2.根据权利要求1所述的一种稀土掺杂硅基薄膜材料，其特征在于，步骤S2中，所述硅基材料选自单晶硅光伏薄膜材料、多晶硅光伏薄膜材料中的一种或两种。
3.根据权利要求1所述的一种稀土掺杂硅基薄膜材料，其特征在于，步骤S2中，多晶材料的用量为0.15~0.55mol，硅基材料的规格为15mm×15mm×（70~85）nm。
4.根据权利要求1所述的一种稀土掺杂硅基薄膜材料，其特征在于，步骤S3中，第一次退火的温度为300~700℃，退火时间为12~18min；第二次退火的温度为1050~1200℃，退火时间为22~28min。
5.根据权利要求1所述的一种稀土掺杂硅基薄膜材料，其特征在于，步骤S3中，稀土离子采用离子注入法注入，真空压力为3×10-3~4×10-3Pa，注入稀土氧化物携带的能量为120~180Kev。
6.根据权利要求1所述的一种稀土掺杂硅基薄膜材料，其特征在于，步骤S3中，稀土离子的注入总剂量为1014~1018ions/cm2。
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