CN110373716B - 一种二维超薄CuBr纳米片的制备方法及其应用 - Google Patents
一种二维超薄CuBr纳米片的制备方法及其应用 Download PDFInfo
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- 229910021589 Copper(I) bromide Inorganic materials 0.000 title claims abstract description 68
- 239000002135 nanosheet Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 239000013078 crystal Substances 0.000 claims abstract description 32
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011889 copper foil Substances 0.000 claims abstract description 17
- 239000010445 mica Substances 0.000 claims abstract description 16
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000010453 quartz Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 7
- 238000011144 upstream manufacturing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000005411 Van der Waals force Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 23
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 abstract description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000012512 characterization method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 239000002055 nanoplate Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 229910052950 sphalerite Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 238000000879 optical micrograph Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical group [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfides Chemical class 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
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Abstract
本发明提供一种二维超薄CuBr纳米片的制备方法及其应用,属于二维纳米材料制备技术领域。通过简单的化学气相沉积法,在云母上通过范得瓦尔斯外延生长,避免了基底与材料的晶格失配;采用BiBr3作为反应源、铜箔作为限域手段,通过调节源量、反应温度和反应时间等参数,得到了厚度为0.9nm~200nm,尺寸为2~150μm的三角形单晶纳米片,实现了CuBr纳米片的可控生长,且制备的CuBr单晶性好,与基底之间不存在晶格失配。
Description
技术领域
本发明属于二维纳米材料制备技术领域,具体涉及一种二维超薄非层状CuBr单晶纳米片的制备方法及其应用。
背景技术
自从2004年石墨烯被安德烈海姆发现以来,众多不同种类不同性质的二维材料,如六方氮化硼,过渡金属硫化物,黑磷等相继被发现并展示出极其优异的电学性质和光学性能。然而,目前二维材料的研究主要局限于具有层状结构的材料,这是因为层状材料的层间范德华接触较弱,可以较为容易地通过机械剥离或CVD等方法制备。但相比于层状材料,非层状材料占据着大多数的材料种类,并且有众多极其重要的半导体材料在属于此列。因此将非层状半导体材料二维化,利用二维材料特性,提升半导体材料的电学和光学性能,并且能够避免晶格失配,有利于构建异质结器件,具有重要意义。然而迄今为止,如何低成本生长超薄高性能的二维非层状材料仍存在着极大的问题。
CuBr是一种具有闪锌矿结构的直接带隙宽禁带半导体材料,室温禁带宽度约为3eV,具有很高的激子结合能108meV和非线性光学的性质,相比于GaN,SiC,ZnO等传统宽禁带半导体,其具有低成本、激子能级丰富和激子结合能大的优势,在发光二极管、紫外光电探测,非线性光学等领域有着广泛的应用前景。但是在过去的块体材料应用中,由于其存在形式多为多晶形式,并且存在与基底的晶格失配的现象,材料缺陷较多,因此制备出来的器件性能往往很差。
发明内容
针对背景技术所存在的不易制备高质量二维非层状CuBr单晶材料的问题,本发明的目的在于提供一种二维超薄CuBr单晶纳米片的制备方法及其应用,该方法通过简单的化学气相沉积法,采用BiBr3作为反应源、铜箔作为限域手段,通过调节源量、反应温度和生长时间控制生成的二维纳米片的厚度和尺寸,且制备的CuBr单晶性好,与基底之间不存在晶格失配。
为实现上述目的,本发明的技术方案如下:
一种二维超薄CuBr单晶纳米片的制备方法,包括以下步骤:
步骤1:将BiBr3粉末置于坩埚中,然后将坩埚放置于石英管上游第一加热区中心;将覆盖铜箔的基片放置于石英管下游第二加热区中心,其中,铜箔与基片的间距为0~100μm;
步骤2:将石英管内部抽真空至0.1Pa以下,通入Ar气使管内气压保持常压环境,然后向管内通入Ar和H2混合气体;
步骤3:将第二加热区升温至275~325℃,保持10~60min后,再将第一加热区升温至200~275℃,反应3~20min,反应结束后自然冷却至室温,取出基片,即可在基片上制备得到所述的CuBr单晶纳米片。
进一步地,步骤1所述基片为具有范德瓦尔斯力的基片,具体为云母或者石墨烯基底等。
进一步地,步骤1所述BiBr3粉末的质量为2~200mg。
进一步地,步骤2所述Ar和H2混合气体中,H2体积占比为0%~10%,混合气体的流速为50~100sccm。
进一步地,步骤3所述第二加热区的升温速率为10~25℃/min;第一加热区的升温速率为15~30℃/min。
本发明还公开了一种采用如上述制备方法得到的CuBr单晶纳米片,厚度为0.9nm~200nm,尺寸为2~150μm。
本发明还提供了上述CuBr单晶纳米片在光电探测器中的应用,器件制备方法为:在所述CuBr单晶纳米片上覆盖掩膜板,然后通过热蒸镀原位沉积银电极,其中电极厚度为25~100nm。
进一步地,所述掩膜板为Ni网、Cu网或Fe网等。
综上所述,由于采用了上述技术方案,本发明的有益效果是:
1.本发明提供的一种超薄二维单晶CuBr纳米片的制备方法,该方法通过简单的化学气相沉积法,采用BiBr3作为反应源、铜箔作为限域手段,通过调节源量、反应温度和反应时间等参数,得到了厚度为0.9nm~200nm,尺寸为2~150μm的三角形单晶纳米片,实现了CuBr纳米片的可控生长。
2.本发明在云母上通过范德瓦尔斯外延生长,避免了基底与材料的晶格失配,得到了高质量的二维单晶CuBr纳米片,可控性强,工艺参数容易控制,安全绿色无污染、产率高。
附图说明
图1为本发明CuBr纳米片的生长装置示意图。
图2为本发明实施例1所制备的CuBr纳米片的光学显微图,右上角插图为对应的AFM表征图。
图3为本发明实施例1所制备的CuBr纳米片的结构和元素表征图;
其中,(a)为XRD图谱以及闪锌矿结构CuBr的pdf卡片,(b)为拉曼图谱,(c)为XPS图谱。
图4为本发明实施例1所制备的CuBr纳米片的光学性能表征图;
其中,(a)为紫外-可见吸收光谱图,(b)为光致发光图谱图,(c)为荧光寿命数据图。
图5基于本发明实施例1所得到的CuBr纳米片制备的光电探测器件在不同光功率下的光响应I-V图。
图6为本发明实施例2所制备的CuBr纳米片的AFM扫描图,右上角插图为对应框内的精细AFM扫描图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面结合实施方式和附图,对本发明作进一步地详细描述。
实施例1
一种二维超薄CuBr单晶纳米片的制备方法,包括以下步骤:
步骤1:将10mg的BiBr3粉末置于Al2O3坩埚中,然后将坩埚放入石英管上游第一加热区中心;在石英板上放置云母基片,在基片上覆盖表面平整的铜箔,控制铜箔与云母基片的间距为50μm,然后将石英板放入石英管下游第二加热区中心;
步骤2:将石英管内部抽真空至0.1Pa以下,通入500sccm的Ar气,以去除管内残余的空气并使管内气压保持常压环境,然后向管内通入H2体积占比5%的Ar/H2混合气体,将气流调整为材料生长所需要的流速50sccm;
步骤3:将第二加热区在15min内升温至325℃,保持15min后,再将第一加热区在10min内加热至200℃,反应5min,反应结束后自然冷却至室温,取出基片,即可在基片上制备得到所述的CuBr单晶纳米片。
一种基于上述CuBr单晶纳米片的光电探测器的制备,包括以下步骤:将具有600目的Ni格栅覆盖在CuBr单晶纳米片上,然后通过热蒸镀的方法将50nm的Ag电极沉积在二维CuBr薄片形成光电探测器件。
实施例1制备的CuBr单晶纳米片的光学显微图如图2所示,结构和元素表征图如图3所示,光学性能表征图如图4所示,基于CuBr单晶纳米片制备的光电探测器件在不同光功率下的光响应I-V图如图5所示。
实施例2
一种二维超薄CuBr单晶纳米片的制备方法,包括以下步骤:
步骤1:将10mg的BiBr3粉末置于Al2O3坩埚中,然后将坩埚放入石英管上游第一加热区中心;在石英板上放置云母基片,在基片上覆盖表面平整的铜箔,控制铜箔与云母基片的间距为0μm,然后将石英板放入石英管下游第二加热区中心;
步骤2:将石英管内部抽真空至0.1Pa以下,通入500sccm的Ar气,以去除管内残余的空气并使管内气压保持常压环境,然后向管内通入H2体积占比5%的Ar/H2混合气体,将气流调整为材料生长所需要的流速50sccm;
步骤3:将第二加热区在15min内升温至325℃,保持15min后,再将第一加热区在10min内加热至220℃,反应5min,反应结束后自然冷却至室温,取出基片,即可在基片上制备得到所述的CuBr单晶纳米片。
实施例2制备的CuBr单晶纳米片的AFM扫描图如图6所示。
实施例3
步骤1:将50mg的BiBr3粉末置于Al2O3坩埚中,然后将坩埚放入石英管上游第一加热区中心,在石英板上放置云母基片,在基片上覆盖表面平整的铜箔,控制铜箔与云母基片的间距为25μm,然后将石英板放入石英管下游第二加热区中心;
步骤2:将石英管内部抽真空至0.1Pa以下,通入500sccm的Ar气,以去除管内残余的空气并使管内气压保持常压环境,然后向管内通入Ar气,将气流调整为材料生长所需要的流速75sccm;
步骤3:将第二加热区在15min内升温至305℃,保持15min后,再将第一加热区在10min内加热至275℃,反应5min,反应结束后自然冷却至室温,取出基片,即可在基片上制备得到所述的CuBr单晶纳米片。
实施例4
按照实施例2的步骤制备CuBr单晶纳米片,仅将步骤1中的铜箔与云母基片的间距调整为100μm,其他步骤不变。
本实施例制备的CuBr单晶纳米片的厚度较厚,可达200nm。
图1为本发明CuBr纳米片的生长装置示意图。本发明在石英管的两个加热温区分别放置Al2O3坩埚和石英板,其中BiBr3源放置于坩埚内,然后置于上游加热区中心,云母衬底上覆盖有铜箔进行反应限域,放置在石英板上,然后置于下游加热区中心;加热时,BiBr3源沿着气流方向进入铜箔与云母的夹缝,与铜箔接触发生反应,沉积于云母上,制备得到所述CuBr纳米片。
图2为实施例1制备的二维CuBr纳米片的光学显微图,从图中可以看出,CuBr纳米片为三角形,厚度在8.8nm,尺寸在4μm,均匀地生在在云母片表面。
图3为本发明实施例1所制备的CuBr纳米片的结构和元素表征图,其中,图3a为二维CuBr纳米片的XRD衍射图谱,可以看到,CuBr纳米片的衍射峰完全符合闪锌矿结构的CuBr的PDF卡片,故生长所得材料为闪锌矿结构的CuBr;图3b为拉曼图谱,其峰位与之前闪锌矿结构的CuBr的拉曼峰位置相符合;图3c为XPS分析数据,图中为Cu2p1/2,Cu2p3/2,Br3d3/2,Br3d5/2四个峰位,并且Cu2p附近没有卫星峰,说明所得CuBr纯度较高,结晶性较好。
图4为本发明实施例1所制备的CuBr纳米片的光学性能表征图,其中,图4a为二维CuBr纳米片的室温激子吸收现象,具有Z1,2和Z3激子的2个主要吸收峰,说明CuBr具有较大的激子结合能,图4b为二维CuBr纳米片在416nm附近的室温激子荧光现象,说明了CuBr具有短波发光器件的应用前景,图4c为二维CuBr纳米片的荧光寿命曲线图,从图中可以看出,材料具有346.59ps的短荧光寿命,说明了CuBr具有较高的晶体质量。
图5为二维CuBr纳米片在不同功率下的345nm紫外光照下光电器件性能,展示了一个在0V下非0电流的器件性能,说明其具有自驱动的紫外光探测性能。
图6为实施例2的生长的CuBr纳米片,该参数制备的纳米片具有45μm边长,厚度可达0.91nm。
以上所述,仅为本发明的具体实施方式,本说明书中所公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换;所公开的所有特征、或所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以任何方式组合。
Claims (6)
1.一种二维超薄CuBr单晶纳米片的制备方法,其特征在于,包括以下步骤:
步骤1:将BiBr3粉末放置于石英管上游第一加热区中心,将覆盖铜箔的基片放置于石英管下游第二加热区中心,其中,所述铜箔与基片的间距为0~100μm;
步骤2:将石英管内部抽真空至0.1Pa以下,通入Ar气使管内气压保持常压环境,然后向管内通入Ar气、或Ar气和H2混合气体;
步骤3:将第二加热区升温至275~325℃,保持10~60min后,再将第一加热区升温至200~275℃,反应3~20min,反应结束后自然冷却至室温,取出基片,即可在基片上制备得到所述的CuBr单晶纳米片。
2.根据权利要求1所述二维超薄CuBr单晶纳米片的制备方法,其特征在于,步骤1所述基片为具有范德瓦尔斯力的基片。
3.根据权利要求2所述二维超薄CuBr单晶纳米片的制备方法,其特征在于,所述具有范德瓦尔斯力的基片为云母或石墨烯基底。
4.根据权利要求1所述二维超薄CuBr单晶纳米片的制备方法,其特征在于,步骤1所述BiBr3粉末的质量为2~200mg。
5.根据权利要求1所述二维超薄CuBr单晶纳米片的制备方法,其特征在于,步骤2所述Ar和H2混合气体中,H2体积占比大于0%并且小于等于10%,混合气体的流速为50~100sccm。
6.根据权利要求1所述二维超薄CuBr单晶纳米片的制备方法,其特征在于,步骤3所述第二加热区的升温速率为10~25℃/min,第一加热区的升温速率为15~30℃/min。
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