WO2018145331A1 - 一种高光致发光性能的石墨烯-多孔硅材料及制备方法 - Google Patents

一种高光致发光性能的石墨烯-多孔硅材料及制备方法 Download PDF

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WO2018145331A1
WO2018145331A1 PCT/CN2017/074496 CN2017074496W WO2018145331A1 WO 2018145331 A1 WO2018145331 A1 WO 2018145331A1 CN 2017074496 W CN2017074496 W CN 2017074496W WO 2018145331 A1 WO2018145331 A1 WO 2018145331A1
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graphene
porous silicon
high photoluminescence
copper foil
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葛道晗
张立强
钱栋梁
程广贵
丁建宁
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Jiangsu University
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    • C09K11/02Use of particular materials as binders, particle coatings or suspension media therefor
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K11/00Luminescent materials, e.g. electroluminescent or chemiluminescent
    • C09K11/08Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials
    • C09K11/59Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials containing silicon
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    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
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    • C25F3/12Etching of semiconducting materials

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  • the invention relates to a nanoporous silicon material in the field of luminescent properties, luminescent materials, light-emitting devices and the like, and belongs to the technical field of photoluminescent materials and materials, in particular to a method for improving the microstructure of porous silicon to enhance its photoluminescence performance, It is a graphene-porous silicon material with high photoluminescence properties and a preparation method.
  • Porous Silicon is a porous silicon material with nanostructure formed by electrochemical etching of silicon wafer. Porous silicon has high electrical resistivity, large specific surface area and high chemical activity, and new progress has been made in porous silicon luminescence. However, porous silicon has always had a problem of low luminous efficiency. How to improve the photoluminescence properties of porous silicon has become one of the urgent concerns.
  • the essential feature is that the graphene and the porous silicon are combined to form a graphene-porous silicon composite microstructure, and the porous silicon is modified by using the excellent optical and electrical properties of the graphene.
  • an n-type silicon wafer is selected, which is ultrasonically cleaned in an anhydrous ethanol solution and deionized water for 20 minutes, respectively, and then blown dry with a nitrogen gun.
  • the silicon wafer is electrochemically etched, and then the prepared composite material is degummed in an acetone solution to obtain a porous silicon composite material having graphene.
  • a graphene-porous silicon material with high photoluminescence properties in which graphene is coated on porous silicon to form a composite structure; photoluminescence properties of the graphene-porous silicon are 7.9 times that of the porous silicon monomer.
  • a method for preparing a graphene-porous silicon material with high photoluminescence properties the steps are as follows:
  • Step 1 Preparing a single layer of graphene on a copper foil by chemical vapor deposition (CVD) to obtain a graphene-covered copper foil;
  • Step 2 selecting materials: selecting an n-type single crystal silicon wafer for double-sided polishing;
  • Step 3 Preparation of porous silicon: the n-type single crystal silicon wafer processed in step 2 is sequentially ultrasonically cleaned in anhydrous ethanol and deionized water, washed and then dried; the blown dry n-type single crystal silicon wafer is in hydrogen. Electrochemical etching in a mixed solution of hydrofluoric acid/anhydrous ethanol, after electrochemical etching is completed, washing with deionized water, and drying to obtain porous silicon;
  • Step 4 Graphene transfer: cutting the graphene-covered copper foil obtained in step 1 to have a size equivalent to that of the porous silicon, and after the cutting is completed, placing the copper foil on the glass sheet; Transfer to the glue machine and point the PMMA glue, transfer the glue to the baking table and bake it; place the baked glass piece in the ammonium persulfate solution to etch the copper foil substrate, every 10 minutes.
  • the ionized water is washed once until the copper foil completely disappears, and the surface of the porous silicon obtained in the step 3 is contacted with the graphene floating on the surface of the ammonium persulfate solution to make the porous silicon surface be combined with the graphene; finally, the graphene is composited with the porous silicon.
  • the material was placed in acetone to remove the glue, and the acetone was changed once every 10 minutes; after the completion of the glue removal, the graphene-porous silicon material having the high photoluminescence property was obtained.
  • the n-type double throwing silicon wafer has a resistance of 3 to 8 ⁇ cm 2 and a thickness of 450 ⁇ m.
  • step 2 the size of the n-type double throwing silicon wafer is 1.6 cm x 1.6 cm.
  • step 3 the ultrasonic cleaning time is 20 min.
  • the volume ratio of hydrofluoric acid to absolute ethanol in the mixed solution of hydrofluoric acid/anhydrous ethanol is 1:1.
  • step 3 the electrochemical corrosion current is 10 to 30 mA, and the etching time is 10 minutes.
  • step 4 the speed of the homogenizer is 4000 r/min.
  • step 4 the baking temperature is 150 ° C and the baking time is 5 min.
  • the ammonium persulfate solution has a concentration of 10 mg to 50 mg/mL.
  • the substrate material used in the present invention is relatively simple, and the apparatus used in the preparation process is simple and easy to handle.
  • the material is relatively reasonably used throughout the preparation process and does not waste.
  • the process of treating the porous silicon surface is simple, and now the graphene preparation process is increasingly mature, and higher quality graphene can be obtained.
  • the preparation process of the entire composite material is short, the overall process steps are easy to operate, the chemical reagents used are less, and the environment is not polluted.
  • this composite structure can increase the photoluminescence properties of porous silicon by several times (about 7.9 times) without affecting other properties of porous silicon.
  • Figure 1 is a schematic view of a graphene-porous silicon structure
  • Figure 2 is an SEM image of a porous silicon microstructure
  • Figure 3 is a graph showing the photoluminescence properties of a graphene-porous silicon material.
  • Examples 1 to 5 in the preparation of graphene, a single-layer graphene was prepared on a copper foil by a conventional chemical vapor deposition (CVD) method to obtain a graphene-covered copper foil.
  • CVD chemical vapor deposition
  • the prepared graphene-porous silicon material was tested by a fluorescence spectrophotometer and found to have a photoluminescence performance of 7.9 times that of a simple porous silicon structure, as shown in FIG.
  • porous silicon The selected samples were ultrasonically washed in absolute ethanol and deionized water for 20 minutes. Thereafter, it was taken out with tweezers and blown dry with a nitrogen gun for use.
  • the prepared silicon wafer was electrochemically etched in a mixed solution of hydrofluoric acid/anhydrous ethanol in a volume ratio of 1:1, the current was set to 30 mA, the etching time was 10 minutes, and after the corrosion was completed, it was washed with deionized water and used. The nitrogen gun was blown dry.
  • porous silicon The selected samples were ultrasonically washed in absolute ethanol and deionized water for 20 minutes. Thereafter, it was taken out with tweezers and blown dry with a nitrogen gun for use.
  • the prepared silicon wafer was electrochemically etched in a mixed solution of hydrofluoric acid/anhydrous ethanol in a volume ratio of 1:1, and the current was set to 30 mA for 10 minutes. After the corrosion was completed, it was washed with deionized water and nitrogen gas was used. The gun is blown dry.
  • the copper foil substrate was etched in ammonium persulfate solution, and the sample was taken out at intervals of 10 minutes and washed with deionized water until the copper foil completely disappeared; then the surface of the porous silicon was contacted with graphene floating on the surface of the ammonium persulfate solution to make the porous silicon The surface is compounded with graphene; finally, the porous silicon and graphene composite materials are placed in acetone to be degummed, and acetone is changed every 10 minutes. After the completion of the degumming, the porous silicon having graphene is taken out to obtain the graphene-porous silicon material having high photoluminescence properties.
  • porous silicon The selected samples were ultrasonically washed in absolute ethanol and deionized water for 20 minutes. Thereafter, it was taken out with tweezers and blown dry with a nitrogen gun for use.
  • the prepared silicon wafer was electrochemically etched in a mixed solution of hydrofluoric acid/anhydrous ethanol in a volume ratio of 1:1, and the current was set to 10 mA for 10 minutes. After the corrosion was completed, it was washed with deionized water and nitrogen gas was used. The gun is blown dry.
  • porous silicon The selected samples were ultrasonically washed in absolute ethanol and deionized water for 20 minutes. Thereafter, it was taken out with tweezers and blown dry with a nitrogen gun for use.
  • the prepared silicon wafer was electrochemically etched in a mixed solution of hydrofluoric acid/anhydrous ethanol in a volume ratio of 1:1, and the current was set to 30 mA for 10 minutes. After the corrosion was completed, it was washed with deionized water and nitrogen gas was used. The gun is blown dry.

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Abstract

本发明提供了一种高光致发光性能的石墨烯-多孔硅材料及制备方法,制备步骤如下:1、通过CVD法在铜箔上制备单层石墨烯,得到有石墨烯覆盖的铜箔;2、选择n型单晶硅片,进行双面抛光;3、将步骤2中处理好的n型单晶硅片依次在无水乙醇、去离子水中超声清洗,清洗后吹干;将吹干的n型单晶硅片在氢氟酸/无水乙醇混合溶液中进行电化学腐蚀,电化学腐蚀完成后用去离子水清洗,并吹干得到多孔硅;4、将石墨烯处理后,使多孔硅表面与石墨烯复合;最后将石墨烯与多孔硅复合的材料置于丙酮中去胶,得到所述的高光致发光性能的石墨烯-多孔硅材料。本发明制备的石墨烯-多孔硅材料,显著提高了多孔硅的光学性能指标,拓宽了其光学应用前景。

Description

一种高光致发光性能的石墨烯-多孔硅材料及制备方法 技术领域
本发明涉及纳米多孔硅材料在发光性能、发光材料、发光器件等相关应用领域,属于光致发光材料和材料复合技术领域,尤其涉及改善多孔硅的微结构增强其光致发光性能的方法,具体为一种高光致发光性能的石墨烯-多孔硅材料及制备方法。
背景技术
多孔硅(Porous Silicon)是硅片经电化学腐蚀而形成的一种具有纳米结构的多孔硅材料。多孔硅具有高电阻率、很大的比表面积及很高的化学活性,多孔硅发光不断有新的进展。但多孔硅一直存在发光效率低的问题。如何提高多孔硅的光致发光特性成为人们迫切关注的问题之一。为克服这这一缺点,人们已经尝试了各种办法,通过对单晶硅表面进行脉冲处理(专利号:CN102260496A);通过烯氢和烯酸对多孔硅进行表面改性处理(专利号:CN103288087A);将多孔硅制备成胶态光致发光非晶形多孔硅粒子悬浮液的方法(专利号:CN104428394A),等等。但一直未发现一种合适的方法或者新型结构来增强多孔硅的光致发光性能。
因此,寻找一种能够简单、高效的多孔硅微结构或者制备工艺,来增强多孔硅光致发光性能的方法,成为目前人们的研究热点。
发明内容
针对现有技术存在的不足,本发明的目的在于,提高多孔硅的光致发光性能。本发明为解决多孔硅光致发光性能低的问题而采用的技术方案为:
将石墨烯转移覆盖于多孔硅之上,形成复合结构;增强其光致发光性能。其本质特征在于:将石墨烯与多孔硅进行复合,形成石墨烯-多孔硅复合微结构,利用石墨烯优异的光、电学特性,对多孔硅进行改性。
本发明选用n型硅片,分别将其在无水乙醇溶液、去离子水中超声清洗20分钟,然后用氮气枪吹干。再对硅片进行电化学腐蚀,之后将制备好的复合材料放在丙酮溶液中去胶,最终得具有石墨烯的多孔硅复合材料。
具体技术方案如下:
一种高光致发光性能的石墨烯-多孔硅材料,所述石墨烯-多孔硅中,石墨烯覆盖于多孔硅之上,形成复合结构;所述石墨烯-多孔硅的光致发光性能是所述多孔硅单体的7.9倍。
一种高光致发光性能的石墨烯-多孔硅材料的制备方法,步骤如下:
步骤1、通过化学气相沉积法(CVD)在铜箔上制备单层石墨烯,得到有石墨烯覆盖的铜箔;
步骤2、选择材料:选择n型单晶硅片,进行双面抛光;
步骤3、多孔硅的制备:将步骤2中处理好的n型单晶硅片依次在无水乙醇、去离子水中超声清洗,清洗后吹干;将吹干的n型单晶硅片在氢氟酸/无水乙醇混合溶液中进行电化学腐蚀,电化学腐蚀完成后用去离子水清洗,并吹干得到多孔硅;
步骤4、石墨烯转移:裁剪步骤1得到的有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上;将所述玻璃片其转移到匀胶机上并点上PMMA胶,完成涂胶后转移到烘胶台上烘烤;将烘烤后的玻璃片置于过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟用去离子水清洗一次,直至铜箔完全消失,再用步骤3得到的多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将石墨烯与多孔硅复合的材料置于丙酮中去胶,间隔10分钟换一次丙酮;去胶完成后,得到所述的高光致发光性能的石墨烯-多孔硅材料。
步骤2中,所述n型双抛硅片电阻为3~8Ω·cm2,厚度为450μm。
步骤2中,所述n型双抛硅片的尺寸为1.6cm×1.6cm。
步骤3中,所述超声清洗的时间为20min。
步骤3中,所述氢氟酸/无水乙醇的混合溶液中,氢氟酸与无水乙醇的体积比为1:1。
步骤3中,所述电化学腐蚀的电流为10~30mA,腐蚀时间为10min。
步骤4中,所述匀胶机的转速为4000r/min。
步骤4中,所述烘烤温度为150℃,烘烤时间为5min。
步骤4中,所述过硫酸铵溶液浓度为10mg~50mg/mL。
有益效果:
(1)本发明中使用的衬底材料相对简单,在制备过程中使用的仪器设备简单,容易操作。在整个制备过程中材料使用相对合理,不产生浪费。对多孔硅表面进行处理的过程简单,而且现在石墨烯制备工艺日益成熟,可以得到质量较高的石墨烯。整个复合材料的制备过程时间较短,整体的工艺步骤容易操作,采用的化学试剂较少,对环境无污染。相比于纯多孔硅的光致发光性能,这种复合结构可以将多孔硅的光致发光性能提高数倍(约7.9倍),并且不影响多孔硅其他的性能。
(2)提出了一种石墨烯-多孔硅材料,显著提高了多孔硅的光学性能指标,拓宽了 其光学应用前景。
(3)针对提出的复合结构,给出了相关的制备工艺流程及关键工艺参数,该方法步骤简单易行,成本低廉,具有很好的工程应用前景。
附图说明
图1为石墨烯-多孔硅结构示意图;
图2为多孔硅微结构SEM图;
图3为石墨烯-多孔硅材料的光致发光性能结果。
图中:1-单晶硅片,2-多孔硅,3-石墨烯
具体实施方式
实施例1~5中,在制备石墨烯时,均通过传统的化学气相沉积法(CVD)在铜箔上制备单层石墨烯,得到有石墨烯覆盖的铜箔。
实施例1:
1.选择材料:选择电阻为3~8Ω.cm2、厚度为450μm且晶向为[100]的n型单晶硅片(双面抛光),尺寸为1.6cm×1.6cm。
2.多孔硅的制备:将上述选好的样品依次在无水乙醇、去离子水中超声清洗20分钟。此后用镊子取出并用氮气枪吹干备用。将准备好的硅片在体积比为1:1的氢氟酸/无水乙醇的混合溶液进行电化学腐蚀,电流设置为10mA、腐蚀时间为10分钟,腐蚀完成后用去离子水清洗,并用氮气枪吹干,如图2所示。
3.石墨烯的转移:裁剪有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上,将其转移到匀胶机上并点上PMMA胶,启动匀胶机将转速设置为4000转每分钟;涂胶完成后转移至烘胶台烘烤,温度设置为150℃,时间为5分钟;此后将其放入浓度为10mg/ml的过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟将样品取出并用去离子水清洗,直至铜箔完全消失;再用多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将多孔硅和石墨烯复合的材料放于丙酮中去胶,每隔10分钟换一次丙酮。去胶完成后,将具有石墨烯的多孔硅取出,得到所述的高光致发光性能的石墨烯-多孔硅材料,如图1所示。
制备出的石墨烯-多孔硅材料,利用荧光分光光度计进行测试发现,其光致发光性能是单纯多孔硅结构的7.9倍,如图3所示。
实施例2:
1.选择材料:选择电阻为3~8Ω.cm2、厚度为450μm且晶向为[100]的n型单晶硅 片(双面抛光),尺寸为1.6cm×1.6cm。
2.多孔硅的制备:将上述选好的样品依次在无水乙醇、去离子水中超声清洗20分钟。此后用镊子取出并用氮气枪吹干备用。将准备好的硅片在体积比为1:1的氢氟酸/无水乙醇的混合溶液进行电化学腐蚀,电流设置为30mA、腐蚀时间为10分钟,腐蚀完成后用去离子水清洗,并用氮气枪吹干。
3.石墨烯的转移:裁剪有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上,将其转移到匀胶机上并点上PMMA胶,启动匀胶机将转速设置为4000转每分钟;涂胶完成后转移至烘胶台烘烤,温度设置为150℃,时间为5分钟;此后将其放入浓度为20mg/ml的过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟将样品取出并用去离子水清洗,直至铜箔完全消失;再用多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将多孔硅和石墨烯复合的材料放于丙酮中去胶,每隔10分钟换一次丙酮。去胶完成后,将具有石墨烯的多孔硅取出,得到所述的高光致发光性能的石墨烯-多孔硅材料。
实施例3:
1.选择材料:选择电阻为3~8Ω.cm2、厚度为450μm且晶向为[100]的n型单晶硅片(双面抛光),尺寸为1.6cm×1.6cm。
2.多孔硅的制备:将上述选好的样品依次在无水乙醇、去离子水中超声清洗20分钟。此后用镊子取出并用氮气枪吹干备用。将准备好的硅片在体积比为1:1的氢氟酸/无水乙醇的混合溶液进行电化学腐蚀,电流设置为30mA、时间为10分钟,腐蚀完成后用去离子水清洗,并用氮气枪吹干。
3.石墨烯的转移:裁剪有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上,将其转移到匀胶机上并点上PMMA胶,启动匀胶机将转速设置为4000转每分钟;涂胶完成后转移至烘胶台烘烤,温度设置为150℃,时间为5分钟;此后将其放入浓度为30mg/ml的过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟将样品取出并用去离子水清洗,直至铜箔完全消失;再用多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将多孔硅和石墨烯复合的材料放于丙酮中去胶,每隔10分钟换一次丙酮。去胶完成后,将具有石墨烯的多孔硅取出,得到所述的高光致发光性能的石墨烯-多孔硅材料。
实施例4:
1.选择材料:选择电阻为3~8Ω.cm2、厚度为450μm且晶向为[100]的n型单晶硅 片(双面抛光),尺寸为1.6cm×1.6cm。
2.多孔硅的制备:将上述选好的样品依次在无水乙醇、去离子水中超声清洗20分钟。此后用镊子取出并用氮气枪吹干备用。将准备好的硅片在体积比为1:1的氢氟酸/无水乙醇的混合溶液进行电化学腐蚀,电流设置为10mA、时间为10分钟,腐蚀完成后用去离子水清洗,并用氮气枪吹干。
3.石墨烯的转移:裁剪有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上,将其转移到匀胶机上并点上PMMA胶,启动匀胶机将转速设置为4000转每分钟;涂胶完成后转移至烘胶台烘烤,温度设置为150℃,时间为5分钟;此后将其放入浓度为40mg/ml的过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟将样品取出并用去离子水清洗,直至铜箔完全消失;再用多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将多孔硅和石墨烯复合的材料放于丙酮中去胶,每隔10分钟换一次丙酮。去胶完成后,将具有石墨烯的多孔硅取出,得到所述的高光致发光性能的石墨烯-多孔硅材料。
实施例5:
1.选择材料:选择电阻为3~8Ω.cm2、厚度为450μm且晶向为[100]的n型单晶硅片(双面抛光),尺寸为1.6cm×1.6cm。
2.多孔硅的制备:将上述选好的样品依次在无水乙醇、去离子水中超声清洗20分钟。此后用镊子取出并用氮气枪吹干备用。将准备好的硅片在体积比为1:1的氢氟酸/无水乙醇的混合溶液进行电化学腐蚀,电流设置为30mA、时间为10分钟,腐蚀完成后用去离子水清洗,并用氮气枪吹干。
3.石墨烯的转移:裁剪有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上,将其转移到匀胶机上并点上PMMA胶,启动匀胶机将转速设置为4000转每分钟;涂胶完成后转移至烘胶台烘烤,温度设置为150℃,时间为5分钟;此后将其放入浓度为50mg/ml的过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟将样品取出并用去离子水清洗,直至铜箔完全消失;再用多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将多孔硅和石墨烯复合的材料放于丙酮中去胶,每隔10分钟换一次丙酮。去胶完成后,将具有石墨烯的多孔硅取出,得到所述的高光致发光性能的石墨烯-多孔硅材料。

Claims (10)

  1. 一种高光致发光性能的石墨烯-多孔硅材料,其特征在于,所述石墨烯-多孔硅中,石墨烯覆盖于多孔硅之上,形成复合结构;所述石墨烯-多孔硅的光致发光性能是所述多孔硅单体的7.9倍。
  2. 一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤如下:
    步骤1、通过化学气相沉积法在铜箔上制备单层石墨烯,得到有石墨烯覆盖的铜箔;
    步骤2、选择材料:选择n型单晶硅片,进行双面抛光;
    步骤3、多孔硅的制备:将步骤2中处理好的n型单晶硅片依次在无水乙醇、去离子水中超声清洗,清洗后吹干;将吹干的n型单晶硅片在氢氟酸/无水乙醇混合溶液中进行电化学腐蚀,电化学腐蚀完成后用去离子水清洗,并吹干得到多孔硅;
    步骤4、石墨烯转移:裁剪步骤1得到的有石墨烯覆盖的铜箔,使其尺寸与所述多孔硅的尺寸相当,裁剪完成后,将铜箔放置在玻璃片上;将所述玻璃片其转移到匀胶机上并点上PMMA胶,完成涂胶后转移到烘胶台上烘烤;将烘烤后的玻璃片置于过硫酸铵溶液中腐蚀铜箔衬底,每间隔10分钟用去离子水清洗一次,直至铜箔完全消失,再用步骤3得到的多孔硅表面接触浮在过硫酸铵溶液表面的石墨烯,使多孔硅表面与石墨烯复合;最后将石墨烯与多孔硅复合的材料置于丙酮中去胶,间隔10分钟换一次丙酮;去胶完成后,得到所述的高光致发光性能的石墨烯-多孔硅材料。
  3. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤2中,所述n型双抛硅片电阻为3~8Ω·cm2,厚度为450μm。
  4. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤2中,所述n型双抛硅片的尺寸为1.6cm×1.6cm。
  5. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤3中,所述超声清洗的时间为20min。
  6. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤3中,所述氢氟酸/无水乙醇的混合溶液中,氢氟酸与无水乙醇的体积比为1:1。
  7. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤3中,所述电化学腐蚀的电流为10~30mA,腐蚀时间为10min。
  8. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤4中,所述匀胶机的转速为4000r/min。
  9. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤4中,所述烘烤温度为150℃,烘烤时间为5min。
  10. 根据权利要求2所述的一种高光致发光性能的石墨烯-多孔硅材料的制备方法,其特征在于,步骤4中,所述过硫酸铵溶液浓度为10mg~50mg/mL。
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