CN105908132A - 一种半导体Cu2ZnTiS4薄膜材料及其制备方法 - Google Patents
一种半导体Cu2ZnTiS4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 36
- 239000004065 semiconductor Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 53
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 239000005361 soda-lime glass Substances 0.000 claims abstract description 14
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 4
- 238000004544 sputter deposition Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
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- 239000007888 film coating Substances 0.000 claims description 3
- 238000009501 film coating Methods 0.000 claims description 3
- 238000005477 sputtering target Methods 0.000 claims description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000010408 film Substances 0.000 abstract description 23
- 238000010521 absorption reaction Methods 0.000 abstract description 2
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- 238000000151 deposition Methods 0.000 abstract description 2
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- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
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- VEUACKUBDLVUAC-UHFFFAOYSA-N [Na].[Ca] Chemical compound [Na].[Ca] VEUACKUBDLVUAC-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001424 field-emission electron microscopy Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5866—Treatment with sulfur, selenium or tellurium
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Abstract
本发明涉及薄膜太阳能电池制备技术领域,特指一种新型半导体Cu2ZnTiS4薄膜材料及其制备方法。采用磁控溅射多靶沉积方法,在钠钙玻璃(SLG)衬底表面采用三靶共溅Cu、Zn、Ti制备CZTi前驱体薄膜;将得到的CZT前躯体薄膜在510℃温度下的H2S气氛中保温2个小时,即制备得到Cu2ZnTiS4半导体薄膜。采用本方法制备得到的Cu2ZnTiS4半导体薄膜是一种厚度为200‑2000nm,光学吸收系数为104cm‑1,载流子类型为P型的,具有延展性的半导体薄膜材料,对于实现薄膜材料完全柔性化具有十分重要的科学意义和工程价值。
Description
技术领域
本发明涉及薄膜太阳能电池制备技术领域,特指一种新型半导体Cu2ZnTiS4薄膜材料及其制备方法。
背景技术
近年来,随着地球上有限的石油和煤炭等不可再生资源的逐渐耗尽,可再生能源的利用与开发显得越来越紧迫,其中,太阳能光伏发电将取之不尽的辐射到地面上的太阳能通过太阳电池等光伏器件的光电转换而源源不断地转变成为电能,已经成为可再生能源中最安全、最环保和最具潜力的竞争者。
目前为止,常见的太阳能电池主要包括硅电池,薄膜电池等等,在薄膜电池中主要分为钙钛矿、CIGS与CZTS等,然而钙钛矿电池具有环境不稳定性,CIGS成本较高,CZTS中Sn的熔点较低,在制备过程中及其容易散失,难于制备。
薄膜电池与硅电池相比其一大优点为易于实现柔性化,然而在现有的制备薄膜电池的材料的厚度较大,基本厚度都达到1um以上,延展性较低,可柔性化程度较低。
发明内容
本发明的目的在于提出了一种新型半导体Cu2ZnTiS4薄膜材料及其制备方法。
所述的新型Cu2ZnTiS4半导体薄膜材料是一种厚度仅为200-2000nm的半导体薄膜材料。
所述的新型Cu2ZnTiS4半导体薄膜材料是一种吸收系数为104cm-1的半导体薄膜材料。
所述的新型Cu2ZnTiS4半导体薄膜材料是一种P型半导体薄膜料。
所述的新型Cu2ZnTiS4半导体薄膜材料是一种具有延展性的半导体薄膜料。
本发明的另一目的是提供一种所述新型Cu2ZnTiS4半导体薄膜的制备方法,具体过程如下:采用磁控溅射多靶沉积方法,在钠钙玻璃(SLG)衬底表面采用三靶共溅Cu、Zn、Ti制备CZTi前驱体薄膜;将得到的CZT前躯体薄膜在510℃温度下的H2S气氛中保温2个小时,即制备得到Cu2ZnTiS4半导体薄膜。
所述的钠钙玻璃依次用碱性溶液,丙酮,乙醇和去离子水超声清洗,干燥后作为溅射衬底。
所述的多靶沉积三元金属前躯体薄膜是将钠钙玻璃衬底放入高真空三靶磁控溅射腔体,工作压强0.5-1.2Pa,采用Cu,Zn,Ti三靶共同溅射得到CZTi三元合金前躯体薄膜。
进一步地,将清洗后的钠钙玻璃放入高真空三靶磁控溅射腔体,以Cu、Zn、Ti作为溅射靶材,Cu与Ti采用直流电源,溅射功率分别为10w与42w,Zn采用射频电源,溅射功率为60w,工作压强0.5-1.2Pa,工作气体采用的为体积浓度为99.999%的氩气,控制溅射时间,得到不同厚度的CZTi前驱体薄膜。
所述的CZT前躯体薄膜硫化退火主要是将已经得到的CZT前躯体薄膜,放入有H2S气氛的高温管式炉中,硫化退火温度为510℃,保持120min。
与现有发明相比,本发明具有以下有益效果:本发明主要采用的是真空制备方法,操作简单,成本低,产业化程度高等优点。采用本方法制备得到的Cu2ZnTiS4半导体薄膜是一种厚度为200-2000nm,光学吸收系数为104cm-1,载流子类型为P型的,具有延展性的半导体薄膜材料,对于实现薄膜材料完全柔性化具有十分重要的科学意义和工程价值。
附图说明
图1为本发明制备的Cu2ZnTiS4半导体薄膜的XRD图。
图2为本发明制备的Cu2ZnTiS4半导体薄膜的SEM图。
图3为本发明制备的Cu2ZnTiS4半导体薄膜的EDS能谱图。
图4为本发明制备的Cu2ZnTiS4半导体薄膜的吸收率图。
图5为本发明制备的Cu2ZnTiS4半导体薄膜的延展性图。
表1为本发明制备的Cu2ZnTiS4半导体薄膜的电学性能表。
表2为本发明制备的Cu2ZnTiS4半导体薄膜的EDS元素比例表。
具体实施方式
下面通过实施例对本发明做进一步详细说明,这些实施例仅用来说明本发明,并不限制本发明的范围
Cu2ZnTiS4半导体薄膜材料是一种厚度为200-2000nm的半导体薄膜材料。
Cu2ZnTiS4半导体薄膜材料是一种吸收系数为104cm-1的半导体薄膜材料。
Cu2ZnTiS4半导体薄膜材料是一种P型半导体薄膜料。
Cu2ZnTiS4半导体薄膜材料是一种具有延展性的半导体薄膜料。
本发明的另一目的是提供一种所述新型Cu2ZnTiS4半导体薄膜的制备方法,具体过程如下:采用磁控溅射多靶沉积方法,在钠钙玻璃衬底表面采用三靶共溅Cu、Zn、Ti制备CZTi前驱体薄膜;将得到的CZT前躯体薄膜在510℃温度下的H2S气氛中保温2个小时,即制备得到Cu2ZnTiS4半导体薄膜。
这些实施例仅用来说明本发明,并不限制本发明的范围
实施例1:
钠钙基底玻璃的清洗
1.衬底选用钠钙玻璃,依次用碱性溶液,丙酮,乙醇,去离子水超声清洗,干燥后备用。
CZTi前驱体薄膜的制备
1.将清洗的钠钙玻璃放入高真空三靶磁控溅射腔体,以Cu、Zn、Ti作为溅射靶材,Cu与Ti采用直流电源,溅射功率分别为10w与42w,Zn采用射频电源,溅射功率为60w,工作压强0.5-1.2Pa,工作气体采用的为体积浓度为99.999%的氩气,溅射时间为15-90min,得到厚度为120-1500nm的前躯体三元金属薄膜。
Cu2ZnTiS4薄膜的制备
1,制备过程需要高温退火,将已经制备得到的CZTi三元金属前躯体薄膜放入石墨盒中,再将石墨盒推入管式炉中心区域,流量为20sccm的H2S气体通入管式炉。
2,炉温以20℃/min的速度升温至510℃,保持120min,在该温度下使前躯体薄膜与H2S气体充分反应进行硫化。
3,自然降温,待100℃以下取出,即制备得新型半导体Cu2ZnTiS4薄膜,制备的样品利用X射线衍射仪进行XRD测试,发现所制备得到的薄膜为锌黄锡矿结构,采用场发射扫描电镜观察薄膜的表面形貌,发现所制备得到的Cu2ZnTiS4薄膜完全结晶,采用EDS能谱仪测量薄膜是否具有四种元素以及元素之比,发现所制备得到的Cu2ZnTiS4薄膜以具有Cu,Zn,Ti,S四种元素,且元素之比为Cu/Zn+Ti=0.88,Zn/Ti=1.07,采用霍尔效应测试其电学性能,发现所制备得到的Cu2ZnTiS4薄膜是一种P型半导体材料,载流子浓度可以达到1020cm-3,光吸收特性由紫外-可见光(UV-VIS)分光光度计测量,发现所制备得到的Cu2ZnTiS4薄膜的吸收系数可以达到104cm-1,采用纳米压痕测试仪测量其是否具有延展性,如图5所示。
表1为本发明制备的Cu2ZnTiS4半导体薄膜的电学性能表
表2为本发明制备的Cu2ZnTiS4半导体薄膜的EDS元素比例表
元素 | 原子比(%) |
Cu | 24 |
Zn | 14 |
Ti | 13 |
S | 49 |
Claims (4)
1.一种半导体Cu2ZnTiS4薄膜材料,其特征在于:所述半导体Cu2ZnTiS4薄膜材料的厚度仅为200-2000nm,吸收系数为104cm-1,是一种P型半导体薄膜料,是一种具有延展性的半导体薄膜料。
2.如权利要求1所述的一种半导体Cu2ZnTiS4薄膜材料的制备方法,其特征在于:采用磁控溅射多靶沉积方法,在钠钙玻璃(SLG)衬底表面采用三靶共溅Cu、Zn、Ti制备CZTi前驱体薄膜;将得到的CZT前躯体薄膜在510℃温度下的H2S气氛中保温2个小时,即制备得到Cu2ZnTiS4半导体薄膜。
3.如权利要求2所述的一种半导体Cu2ZnTiS4薄膜材料的制备方法,其特征在于:所述的钠钙玻璃依次用碱性溶液,丙酮,乙醇和去离子水超声清洗,干燥后作为溅射衬底。
4.如权利要求2所述的一种半导体Cu2ZnTiS4薄膜材料的制备方法,其特征在于:所述的三靶共溅Cu、Zn、Ti制备前躯体薄膜是将清洗后的钠钙玻璃放入高真空三靶磁控溅射腔体,以Cu、Zn、Ti作为溅射靶材,Cu与Ti采用直流电源,溅射功率分别为10w与42w,Zn采用射频电源,溅射功率为60w,工作压强0.5-1.2Pa,工作气体采用的为体积浓度为99.999%的氩气,控制溅射时间,得到不同厚度的CZTi前驱体薄膜。
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