CN105679652A - 一种制备nc-Si/SiOx薄膜MIS结构器件的方法 - Google Patents
一种制备nc-Si/SiOx薄膜MIS结构器件的方法 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 40
- 229910021423 nanocrystalline silicon Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 53
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000005273 aeration Methods 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910001868 water Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- -1 oxygen ions Chemical class 0.000 abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910007991 Si-N Inorganic materials 0.000 abstract description 2
- 229910006294 Si—N Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 210000002381 plasma Anatomy 0.000 abstract 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 23
- 239000007789 gas Substances 0.000 description 10
- 229910003828 SiH3 Inorganic materials 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- OLRJXMHANKMLTD-UHFFFAOYSA-N silyl Chemical compound [SiH3] OLRJXMHANKMLTD-UHFFFAOYSA-N 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 235000013842 nitrous oxide Nutrition 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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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
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Abstract
本发明提供一种制备nc-Si/SiOx薄膜MIS结构器件的方法，所述方法包括：样品制备步骤、样品准备步骤、抽真空步骤、通气步骤、射频发生步骤、加偏压步骤、薄膜生长步骤等。本发明通过加衬底负偏压控制等离子体的能量和离子流密度，增大了N2O分解的氧离子和Si结合速率同时抑制了氮粒子和Si的结合，避免和衬底上的硅活性基团生成Si-N键，减少膜中载流子陷阱的形成，从而提高薄膜的载流子输运效率。
Description
技术领域
本发明涉及一种nc-Si/SiOx薄膜MIS结构器件的方法。
背景技术
纳米晶硅(nc-Si)因量子限制效应而具有一系列独特的光电性能,在全色显示和光伏器件等领域具有诱人的应用前景,通常nc-Si材料采用以SiO2或SiOX为介质的镶嵌结构,相比于SiO2，SiOX作为镶嵌结构具有很多优点，比如有更低的表面态密度，更高的介电常数，而且SiOX带隙可以通过X值调节。这些优点使得nc-Si/SiOx薄膜在异质结中具有更广泛的应用前景。
PECVE法沉积SiOX薄膜通常采用SiH4和N2O作为气体源。X值的调节通过改变SiH4和N2O的馈入比例即可实现。当N2O和SiH4被电离后硅烷与氧离子的动能基本保持一致，容易结合形成SiOx，而氮离子动能均比氧离子和硅烷衰减快，加之大量氮离子已经在N2O开始电离产生的氧离子重新结合生成一氧化氮(NO)挥发气体被排除，因此氮离子再与硅烷发生碰撞反应的概率较低。但是还会残存一部分N离子进入到SiOx薄膜。残存的这部分N会对薄膜的性质产生影响，使得薄膜缺陷增加，影响其电输运，最终导致薄膜光电效率减弱。因此，消除N原子掺入是提高nc-Si/SiOx薄膜质量关键的环节。
发明内容
鉴于现有技术中的上述问题，提出了本发明,本发明的目的在于以SiH4和N2O为反应源用PECVD法生长nc-Si/SiOx薄膜过程中，通过加衬底负偏压控制等离子体的能量和离子流密度。增大了N2O分解的氧离子和Si结合速率同时抑制了氮粒子和Si的结合，避免和衬底上的硅活性基团生成Si-N键，减少膜中载流子陷阱的形成，从而提高薄膜的载流子输运效率。
根据本发明的一方面，提供一种制备nc-Si/SiOx薄膜MIS结构器件的方法，其中，MIS结构器件的M层为电极层，I层为nc-Si/SiOx薄膜，S层为P型晶体硅，其特征在于，所述方法包括以下步骤：(1)样品制备步骤：将双面抛光的P型(100)晶相单晶硅片裁成3cm×3cm见方小片，作为待生长薄膜的衬底，所述单晶硅的电阻率为5-10Ω·cm；(2)样品准备步骤：将单晶硅片先用丙酮和甲醇混合液浸泡3分钟，然后烘干，再用体积比为1:2:5的NH4OH:H2O2:H2O混合液浸泡5分钟，经去离子水处理后，再放入体积比为1:10的HF:H2O溶液中1分钟，然后取出，用去离子水清洗，最后烘干；(3)抽真空步骤；将单晶硅片衬底放在下电极上，进行抽真空，腔内真空度达到10-4pa时加热下电极，加热温度为200-500℃；(4)通气步骤：通入纯度为99.9999％的SiH4气体、纯度为99.999％的H2气体和纯度99.999％的N2O气体的混合气体，其中SiH4、H2和N2O总流量90sccm-150sccm，流量比为2:98:2-2:98:10，反应气压为100-300pa；(5)射频发生步骤：开启射频电源，调节最佳匹配，其中射频电源频率为13.56Mz，功率为80-200w；(6)加偏压步骤：开启下电极偏压源，直流负偏压，电压值为10-100v；(7)薄膜生长步骤：生长nc-Si/SiOx薄膜，生长时间为1-2小时，膜厚为200nm-300nm；以及(8)将生长有nc-Si/SiOx薄膜的单晶硅片取出，放入高真空电阻蒸发镀膜机，并将铝条放入所述镀膜机，打开机械泵腔内压强先抽到5.5pa然后打开分子泵和冷却水将压强抽到10-4帕，再继续抽1小时后开始镀电极膜层，蒸发电压1.45V，镀膜时间为5分钟，镀膜完成后，将nc-Si/SiOx薄膜MIS结构器件取出，测量器件的电学性质。
作为优选的方案，在所述抽真空步骤中，下电极的加热温度为350℃。
作为优选的方案，在所述通气步骤中，SiH4、H2和N2O总流量为104sccm。
作为优选的方案，在所述通气步骤中，SiH4、H2和N2O的流量比为2:98:4。
作为优选的方案，在所述通气步骤中，所述反应气压为230pa。
作为优选的方案，在所述加偏压步骤中，直流负偏压的电压值为65v。
作为优选的方案，在所述射频发生步骤中，射频电源的功率为120w。
作为优选的方案，在所述生长步骤中，氢化纳米晶硅薄膜的厚度控制为200纳米，生长时间为1小时。
附图说明
图1为制备nc-Si/SiOx薄膜MIS结构器件的装置的结构示意图。
具体实施方式
现在，参照附图详细说明本发明的示例性实施例。应当指出，除非另外具体说明，在这些实施例中描述的部件、数字表示和数值的相对配置不限制本发明的范围。
首先，参照图1说明本发明的制备nc-Si/SiOx薄膜MIS结构器件的方法。附图标记说明如下：
1射频阴极；2下电极；3进气口；4出气口；5样品；
6金属反应腔
本发明制备设备包括射频阴极1、下电极2、进气口3、排气口4、样品5和金属反应腔6。
将SiH4、H2和N2O的混合气体从进气口3通入金属反应腔，未反应完的SiH4、H2和N2O及中间产物N2,NO等气体，从排气口5排出。射频阴极1与下电极2之间的距离为5cm，样品5放置于下电极2上。
直流偏压源为下电极2提供直流偏压。偏压为直流负偏压，电压值为10-100v，优选65v。
样品5为单晶硅片，表面积3cm×3cm，厚度0.1mm。
在制备nc-Si/SiOx薄膜时，在射频阴极1和下电极2之间形成等离子放电区，样品5位于等离子放电区内。
接下来，说明nc-Si/SiOx薄膜的形成过程。
首先笑气N2O在等离子体中被分解，产生氧原子或氧自由基，被激活的氧基或者与SiH反应，生成(SiH3)2O，或者参与表面形成氧化物。反应过程为：
N2O+X*→NO+N*
NO+X*→O*+N*
SiH4+O*→(SiH3)2O+H2
(SiH3)2O+O*→SiO2+H2+H2O
其中，X*表示等离子体中的自由基或电子。
下面具体说明本发明的制备nc-Si/SiOx薄膜MIS结构器件的方法，其中M层为电极层，优选为银电极层，I层为nc-Si/SiOx薄膜，S层为P型晶体硅。该方法包括以下步骤：
(1)样品制备步骤：将双面抛光的P型(100)晶相单晶硅片裁成3cm×3cm见方小片，作为待生长薄膜的衬底，所述单晶硅的电阻率为5-10Ω·cm；
(2)样品准备步骤：将单晶硅片衬底先用丙酮和甲醇混合液浸泡3分钟，然后烘干，再用体积比为1:2:5的NH4OH:H2O2:H2O混合液浸泡5分钟，经去离子水处理后，再放入HF:H2O(1:10)中1分钟，然后取出，用去离子水清洗，最后烘干；
(3)抽真空步骤；将单晶硅片衬底放在下电极上，进行抽真空，腔内真空度达到10-4pa时加热下电极，加热温度为200-500℃，优选350℃。(4)通气步骤：通入反应气体SiH4(纯度99.9999％)、H2(纯度99.999％)和N2O(纯度99.999％)的混合气体，其中SiH4、H2和N2O总流量90sccm-150sccm，优选104sccm，流量比2:98:2--2:98:10，优选2:98:4，反应气压为100--300pa，优选230pa；
(5)射频发生步骤：开启射频电源，调节最佳匹配，其中射频电源频率为13.56Mz，功率为80-200w，优选120w。
(6)加偏压步骤：开启下电极偏压源，直流负偏压，电压值为10-100v，优选65v。
(7)薄膜生长步骤：生长nc-Si/SiOx薄膜，生长时间为1-2小时，膜厚为200nm-300nm，膜厚优选为200nm，生长时间优选为1小时。
(8)将生长有nc-Si/SiOx薄膜的单晶硅片取出，放入高真空电阻蒸发镀膜机，并将铝条放入所述镀膜机，打开机械泵腔内压强先抽到5.5pa然后打开分子泵和冷却水将压强抽到10-4帕，再继续抽1小时后开始镀电极膜层，蒸发电压1.45V，镀膜时间为5分钟，镀膜完成后，将nc-Si/SiOx薄膜MIS结构器件取出，测量器件的电学性质。
本发明制备的nc-Si/SiOx薄膜MIS结构器件，通过衬底直流偏压的控制减小了等离子中N离子进入薄膜的几率，降低了薄膜缺陷态形成，提高了MIS器件载流子传输效率。
Claims (8)
1.一种制备nc-Si/SiOx薄膜MIS结构器件的方法，其中，MIS结构器件的M层为电极层，I层为nc-Si/SiOx薄膜，S层为P型晶体硅，其特征在于，所述方法包括以下步骤：
(1)样品制备步骤：将双面抛光的P型(100)晶相单晶硅片裁成3cm×3cm见方小片，作为待生长薄膜的衬底，所述单晶硅的电阻率为5-10Ω·cm；
(2)样品准备步骤：将单晶硅片先用丙酮和甲醇混合液浸泡3分钟，然后烘干，再用体积比为1:2:5的NH4OH:H2O2:H2O混合液浸泡5分钟，经去离子水处理后，再放入体积比为1:10的HF:H2O溶液中1分钟，然后取出，用去离子水清洗，最后烘干；
(3)抽真空步骤；将单晶硅片衬底放在下电极上，进行抽真空，腔内真空度达到10-4pa时加热下电极，加热温度为200-500℃；
(4)通气步骤：通入纯度为99.9999％的SiH4气体、纯度为99.999％的H2气体和纯度99.999％的N2O气体的混合气体，其中SiH4、H2和N2O总流量90sccm-150sccm，流量比为2:98:2-2:98:10，反应气压为100-300pa；
(5)射频发生步骤：开启射频电源，调节最佳匹配，其中射频电源频率为13.56Mz，功率为80-200w；
(6)加偏压步骤：开启下电极偏压源，直流负偏压，电压值为10-100v；
(7)薄膜生长步骤：生长nc-Si/SiOx薄膜，生长时间为1-2小时，膜厚为200nm-300nm；以及
(8)将生长有nc-Si/SiOx薄膜的单晶硅片取出，放入高真空电阻蒸发镀膜机，并将铝条放入所述镀膜机，打开机械泵，腔内压强先抽到5.5pa然后打开分子泵和冷却水将压强抽到10-4帕，再继续抽1小时后开始镀电极膜层，蒸发电压1.45V，镀膜时间为5分钟，镀膜完成后，将nc-Si/SiOx薄膜MIS结构器件取出，测量器件的电学性质。
2.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述抽真空步骤中，下电极的加热温度为350℃。
3.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述通气步骤中，SiH4、H2和N2O总流量为104sccm。
4.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述通气步骤中，SiH4、H2和N2O的流量比为2:98:4。
5.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述通气步骤中，所述反应气压为230pa。
6.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述加偏压步骤中，直流负偏压的电压值为65v。
7.根据权利要求1所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述射频发生步骤中，射频电源的功率为120w。
8.根据权利要求1-7所述的制备nc-Si/SiOx薄膜MIS结构器件的方法，其特征在于，在所述生长步骤中，氢化纳米晶硅薄膜的厚度控制为200纳米，生长时间为1小时。
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