CN110699660A - 在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法 - Google Patents
在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法 Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 57
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000758 substrate Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000010408 film Substances 0.000 claims description 56
- 239000010949 copper Substances 0.000 claims description 23
- 229910052802 copper Inorganic materials 0.000 claims description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 150000002500 ions Chemical class 0.000 claims description 10
- 229920001021 polysulfide Polymers 0.000 claims description 10
- 239000005077 polysulfide Substances 0.000 claims description 10
- 150000008117 polysulfides Polymers 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 229910052977 alkali metal sulfide Inorganic materials 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- DVFCKJNTIQZOPZ-UHFFFAOYSA-N [S-2].[Fr+].[Fr+] Chemical compound [S-2].[Fr+].[Fr+] DVFCKJNTIQZOPZ-UHFFFAOYSA-N 0.000 claims description 2
- QTNDMWXOEPGHBT-UHFFFAOYSA-N dicesium;sulfide Chemical compound [S-2].[Cs+].[Cs+] QTNDMWXOEPGHBT-UHFFFAOYSA-N 0.000 claims description 2
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- AHKSSQDILPRNLA-UHFFFAOYSA-N rubidium(1+);sulfide Chemical compound [S-2].[Rb+].[Rb+] AHKSSQDILPRNLA-UHFFFAOYSA-N 0.000 claims description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000001000 micrograph Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,属于纳米材料技术领域,该方法首先在密封、水存在条件下利用单质硫和碱金属硫化物通过水热反应制得含多硫离子水溶液,然后将铜基底或镀铜膜的其它任意基底放入含多硫离子水溶液中反应,其中含多硫离子水溶液中多硫离子的摩尔浓度为0.1 mol/L~1 mol/L,反应完成后,采用去离子水冲洗干净,干燥,即在任意基底上制得硫化亚铜纳米片阵列薄膜;本发明硫化亚铜纳米片阵列薄膜可在任意基底上进行制备,大大增加了硫化亚铜纳米片阵列薄膜的应用领域和适用性。
Description
技术领域
本发明涉及一种在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,属于纳米材料技术领域。
背景技术
硫化亚铜是一种p型半导体,带隙约1.2 eV,由于其窄的带隙可对太阳光进行有效吸收,能够有效产生光生载流子——电子空穴对,具有优异的光、电、磁以及其他物理化学性质,因此硫化亚铜纳米材料被广泛应用于LED发光二极管、太阳能电池、光电传感器和生物传感器等领域,备受关注与研究。目前,制备硫化亚铜纳米片阵列薄膜的方法众多,如水热法、化学气相沉积等,但这些方法存在一些缺点,如它们都难以大量、可重复地制备硫化亚铜纳米片阵列薄膜,此外,水热法可控性不高且难以在任意基底上生长硫化亚铜纳米片阵列薄膜,化学气相沉积难以制备几百纳米厚度以上的硫化亚铜纳米片阵列薄膜,并且化学气相沉积对设备要求高。因此,需要设计开发一种膜厚可控、易大量、易重复且能在任意基底上制备硫化亚铜纳米片阵列薄膜的方法。
发明内容
本发明针对现有技术存在的部分问题,提供一种在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,这种方法操作简单、膜厚可控,特别地,它可在任意基底上生长硫化亚铜纳米片阵列薄膜。
本发明方法是以单质硫、碱金属硫化物、去离子水和任意基底作为原材料,首先在密封、水存在条件下利用单质硫和碱金属硫化物通过水热反应制得含多硫离子水溶液,然后将铜基底或镀铜膜的其它任意基底放入含多硫离子水溶液中反应,其中含多硫离子水溶液中多硫离子的摩尔浓度为0.1 mol/L~1 mol/L,反应完成后,采用去离子水冲洗干净,干燥,即在任意基底上制得硫化亚铜纳米片阵列薄膜。
所述碱金属硫化物为硫化锂、硫化钠、硫化钾、硫化铷、硫化铯、硫化钫中的一种。
所述水热反应的温度为100 ℃~200 ℃,反应时间1 h以上。
所述镀铜膜的其它基底是指导电或不导电、柔性或非柔性的非铜基底,并在非铜基底上用磁控溅射方法镀铜膜获得,且厚度为几百纳米至几十微米。
所述多硫离子为Sn -2,其中n≥2,其制备过程为(n-1)S+A2S→A2Sn,其中n≥2,A为碱金属元素。
本发明的有益效果是:
(1)本发明以单质硫、碱金属硫化物、去离子水和任意基底(可包括铜基底,以及其他导电或不导电、柔性或非柔性的非铜基底)几种简单原材料,在温和条件下、在任意基底上制得硫化亚铜纳米片阵列薄膜,该方法膜厚可控、易重复和大量制备;
(2)本发明硫化亚铜纳米片阵列薄膜可在任意基底上进行可控制备,大大增加了硫化亚铜纳米片阵列薄膜的应用领域和适用性;
(3)本发明方法操作简单,制备过程易控制,生产成本低廉且环保,适用于工业化大量生产。
附图说明
图1为实施例3硫化亚铜纳米片阵列薄膜的Raman图谱;
图2为实施例3硫化亚铜纳米片阵列薄膜的EDS结果;
图3为实施例1硫化亚铜纳米片阵列薄膜的扫描电镜图;
图4为实施例2硫化亚铜纳米片阵列薄膜的扫描电镜图;
图5为实施例3硫化亚铜纳米片阵列薄膜的扫描电镜图;
图6为实施例4硫化亚铜纳米片阵列薄膜的扫描电镜图;
图7为实施例5硫化亚铜纳米片阵列薄膜的扫描电镜图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1:在导电石墨纸上制备硫化亚铜纳米片阵列薄膜的方法,具体步骤如下:
将15 mmol单质硫(S)和5 mmol硫化钠(Na2S)混合,加入去离子水(H2O)至50 mL,然后将其密封于100 mL水热釜中在100 ℃保温1 h,制得含S4 -2水溶液(S4 -2的摩尔浓度为0.1mol/L),冷却至室温。然后,在2 cm×2 cm×0.1 mm的导电石墨纸上利用磁控溅射技术镀上约4 μm厚的铜膜,再放入含S4 -2水溶液反应2 s,随后立即用去离子水轻轻冲洗干净,干燥后,即在导电石墨纸上制得硫化亚铜纳米片阵列薄膜。
本实施例硫化亚铜纳米片阵列薄膜的扫描电镜图见图3,从图3可知,硫化亚铜纳米片阵列垂直于导电石墨纸竖直生长,整体形貌较均匀。
实施例2:在不导电普通A4打印纸上制备硫化亚铜纳米片阵列薄膜的方法,具体步骤如下:
将30 mmol单质硫(S)和10 mmol硫化钠(Na2S)混合,加入去离子水(H2O)至50 mL,然后将其密封于100 mL水热釜中在200 ℃保温2 h,制得含S4 -2水溶液(S4 -2的摩尔浓度为0.2mol/L),并冷却至室温。然后,在2 cm×2 cm×0.1 mm的不导电A4白纸上利用磁控溅射技术镀上约4 μm的铜膜,放入含S4 -2水溶液反应20 s,随后立即用去离子水轻轻冲洗干净,干燥后,即在不导电普通A4打印纸上制得硫化亚铜纳米片阵列薄膜。
本实施例硫化亚铜纳米片阵列薄膜的扫描电镜图见图4,从图4可知,硫化亚铜纳米片阵列形貌整体较均匀,纳米片长约2 μm,纳米片高(即膜厚)约0.9 μm。
实施例3:硫化亚铜纳米片阵列薄膜的制备方法,具体步骤如下:
将30 mmol单质硫(S)和10 mmol硫化钠(Na2S)混合,加入去离子水(H2O)至50 mL,然后将其密封于100 mL水热釜中在150 ℃保温1.5 h,制得含S4 -2水溶液(S4 -2的摩尔浓度为0.2mol/L),冷却至室温。然后,将2 cm×2 cm×0.3 mm铜片放入含S4 -2水溶液反应40 s,随后立即用去离子水轻轻冲洗干净,干燥后,即在铜片上快速生长出了硫化亚铜纳米片阵列薄膜。
本实施例硫化亚铜纳米片阵列薄膜的扫描电镜图见图5,从图5可知,硫化亚铜纳米片阵列形貌整体较均匀,纳米片长约2.4 μm,纳米片高(即膜厚)约2.4 μm;图1的Raman图谱显示制备的薄膜为Cu2S;图2的EDS结果显示制备的薄膜所含元素为S和Cu(以及微量的O和C,它们来自于薄膜里的结晶水和薄膜表面吸附的CO2)。
实施例4:硫化亚铜纳米片阵列薄膜的制备方法,具体步骤如下:
将30 mmol单质硫(S)和10 mmol硫化钠(Na2S)混合,加入去离子水(H2O)至50 mL,然后将其密封于100 mL水热釜中在150 ℃保温1.5 h,制得含S4 -2水溶液(S4 -2的摩尔浓度为0.2mol/L),并冷却至室温。然后,将2 cm×2 cm×0.3 mm铜片放入含S4 -2水溶液反应80 s,随后立即用去离子水轻轻冲洗干净,干燥后,即在铜片上快速生长出了硫化亚铜纳米片阵列薄膜。
本实施例硫化亚铜纳米片阵列薄膜的扫描电镜图见图6,从图6可知,硫化亚铜纳米片阵列形貌整体较均匀,纳米片长约4 μm,纳米片高(即膜厚)约4.2 μm。
实施例5:硫化亚铜纳米片阵列薄膜的制备方法,具体步骤如下:
将150 mmol单质硫(S)和50 mmol硫化钠(Na2S)混合,加入去离子水(H2O)至50 mL,然后将其密封于100 mL水热釜中在150 ℃保温1.5 h,制得含S4 -2水溶液(S4 -2的摩尔浓度为1mol/L),冷却至室温。然后,将2 cm×2 cm×0.3 mm铜片放入含S4 -2水溶液反应40 s,随后立即用去离子水轻轻冲洗干净,干燥后,即在铜片上快速生长出了硫化亚铜纳米片阵列薄膜。在这种条件下生长出的薄膜易局部脱落。
本实施例硫化亚铜纳米片阵列薄膜的扫描电镜图见图7,从图7可知,硫化亚铜纳米片阵列形貌整体较均匀,纳米片宽约7.4 μm,纳米片高(即膜厚)约8.6 μm。
Claims (5)
1.一种在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,其特征在于:首先在密封、水存在条件下利用单质硫和碱金属硫化物通过水热反应制得含多硫离子水溶液,然后将铜基底或镀铜膜的其它任意基底放入含多硫离子水溶液中反应,其中含多硫离子水溶液中多硫离子的摩尔浓度为0.1 mol/L~1 mol/L,反应完成后,采用去离子水冲洗干净,干燥,即在任意基底上制得硫化亚铜纳米片阵列薄膜。
2.根据权利要求1所述的在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,其特征在于:水热反应的温度为100 ℃~200 ℃,反应时间1 h以上。
3.根据权利要求1所述的在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,其特征在于:碱金属硫化物为硫化锂、硫化钠、硫化钾、硫化铷、硫化铯、硫化钫中的一种。
4.根据权利要求1所述的在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,其特征在于:镀铜膜的其它任意基底是在非铜基底上用磁控溅射方法镀铜膜获得。
5.根据权利要求1所述的在任意基底上快速生长硫化亚铜纳米片阵列薄膜的方法,其特征在于:多硫离子为 Sn -2,其中n≥2。
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CN111718507A (zh) * | 2020-06-10 | 2020-09-29 | 暨南大学 | 一种基于3d打印的超疏水超亲水水分收集装置及其制作方法 |
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CN117747311B (zh) * | 2024-02-20 | 2024-05-28 | 苏州宝丽迪材料科技股份有限公司 | 一种硫化亚铜/碳纳米管纤维电极及其制备方法和应用 |
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