CN107083532A - A kind of preparation method of CuI nanostructure - Google Patents
A kind of preparation method of CuI nanostructure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002086 nanomaterial Substances 0.000 title abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 7
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000010409 thin film Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims 2
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011630 iodine Substances 0.000 abstract description 4
- 229910052740 iodine Inorganic materials 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 2
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- -1 iodide ions Chemical class 0.000 description 1
- 230000026045 iodination Effects 0.000 description 1
- 238000006192 iodination reaction Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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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
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- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
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Abstract
本发明涉及一种CuI纳米结构的制备方法，包括如下步骤：清洗单晶硅衬底的表面，将其装入电子束蒸发装置的真空生长室中；采用电子束蒸发法在单晶硅表面生长一层铜薄膜；将所得的硅基铜薄膜悬挂于反应釜内，水平置于溶液上方，反应釜内的前驱溶液为CuCl2、聚乙烯吡咯烷酮及KI的混合水溶液；将反应釜密封后置于鼓风干燥箱内，于120～200℃条件下水热反应；反应完毕后将样品取出，清洗，吹干。本发明首次利用Cu薄膜和水热合成蒸发出的碘蒸气作为反应原材料，在低温高压条件下制备出大面积均匀的CuI纳米材料，制备工艺与光电器件制备工艺兼容。
The invention relates to a method for preparing a CuI nanostructure, comprising the following steps: cleaning the surface of a single crystal silicon substrate, and putting it into a vacuum growth chamber of an electron beam evaporation device; growing on the surface of a single crystal silicon by electron beam evaporation A layer of copper film; hang the obtained silicon-based copper film in the reactor, and place it horizontally above the solution. The precursor solution in the reactor is a mixed aqueous solution of CuCl 2 , polyvinylpyrrolidone and KI; seal the reactor and place it in In the blast drying oven, hydrothermal reaction is carried out under the condition of 120-200 ℃; after the reaction, the sample is taken out, cleaned and dried. For the first time, the present invention uses Cu film and iodine vapor evaporated by hydrothermal synthesis as reaction raw materials to prepare large-area and uniform CuI nanomaterials under low temperature and high pressure conditions, and the preparation process is compatible with the preparation process of optoelectronic devices.
Description
技术领域technical field
本发明涉及一种CuI纳米结构的制备方法，属于半导体材料技术领域。The invention relates to a preparation method of a CuI nanostructure, which belongs to the technical field of semiconductor materials.
背景技术Background technique
CuI是一种直接带隙宽禁带半导体材料，禁带宽度为3.1eV，激子束缚能高达约62meV。CuI材料在可见光区具有较高的透过率(80％)。由于CuI材料一般存在过剩的碘离子而造成铜空位缺陷，因此表现出p型导电性，且具有较高的空穴迁移率(>40cm2V-1s-1)。此外，CuI还具有无毒、储量丰富、成本低廉的优点。这些优点使得CuI材料在太阳能电池、光电探测器、光电学传感器、显示器件及透明导电薄膜领域表现出广泛的应用前景。CuI is a wide-bandgap semiconductor material with direct bandgap, the bandgap width is 3.1eV, and the exciton binding energy is as high as about 62meV. The CuI material has a high transmittance (80%) in the visible light region. Because CuI materials generally have excess iodide ions and cause copper vacancy defects, they exhibit p-type conductivity and high hole mobility (>40cm 2 V -1 s -1 ). In addition, CuI has the advantages of non-toxicity, abundant reserves, and low cost. These advantages make CuI materials show broad application prospects in the fields of solar cells, photodetectors, photoelectric sensors, display devices and transparent conductive films.
目前，人们利用多种方法实现了CuI薄膜及纳米结构的制备，其中包括真空热蒸发技术、磁控溅射、脉冲激光沉积等物理方法。然而这些制备技术存在真空条件较高、设备操作复杂、制备温度高等缺点。此外，人们还研究了(电)化学合成、高温碘化及溶胶凝胶等化学制备方法来制备CuI薄膜或纳米结构，这些技术尽管设备简单，但存在反应时间长、操作复杂等缺点。B.A.Nejand等人利用一种水热蒸发法制备了CuI纳米结构(MaterialsLetters 132(2014)138-140)，这种方法制备温度较低、反应时间短且材料结晶质量较高，但存在材料生长不均匀的缺点，不能满足大面积器件应用需要。At present, people have realized the preparation of CuI thin films and nanostructures by various methods, including vacuum thermal evaporation technology, magnetron sputtering, pulsed laser deposition and other physical methods. However, these preparation technologies have disadvantages such as high vacuum conditions, complicated equipment operation, and high preparation temperature. In addition, people have also studied chemical preparation methods such as (electro)chemical synthesis, high-temperature iodination, and sol-gel to prepare CuI thin films or nanostructures. Although these technologies have simple equipment, they have disadvantages such as long reaction time and complicated operation. B.A.Nejand et al. used a hydrothermal evaporation method to prepare CuI nanostructures (MaterialsLetters 132 (2014) 138-140). This method has low preparation temperature, short reaction time and high material crystallization quality, but there are problems with material growth. The disadvantage of uniformity cannot meet the needs of large-area device applications.
发明内容Contents of the invention
本发明针对现有CuI纳米结构制备方法上存在的不足，提供一种CuI纳 米结构的制备方法。The present invention aims at the deficiencies in the existing CuI nanostructure preparation method, and provides a kind of CuI nanostructure preparation method.
本发明解决上述技术问题的技术方案如下：The technical scheme that the present invention solves the problems of the technologies described above is as follows:
一种CuI纳米结构的制备方法，其特征在于，包括如下步骤：A preparation method of CuI nanostructure, is characterized in that, comprises the steps:
1)清洗单晶硅衬底的表面，将其装入电子束蒸发装置的真空生长室中；1) cleaning the surface of the single crystal silicon substrate, and putting it into the vacuum growth chamber of the electron beam evaporation device;
2)采用电子束蒸发法在单晶硅表面生长一层铜薄膜；2) growing a layer of copper film on the surface of single crystal silicon by electron beam evaporation;
3)将步骤2)中所得的硅基铜薄膜悬挂于反应釜内，水平置于溶液上方，反应釜内的前驱溶液为CuCl2、聚乙烯吡咯烷酮及KI的混合水溶液；3) Suspend the silicon-based copper film obtained in step 2) in the reactor, and place it horizontally above the solution. The precursor solution in the reactor is a mixed aqueous solution of CuCl 2 , polyvinylpyrrolidone and KI;
4)将步骤3)中的反应釜密封后置于鼓风干燥箱内，于120～200℃条件下水热反应；4) Seal the reaction kettle in step 3) and place it in a blast drying oven, and conduct a hydrothermal reaction at 120-200°C;
5)反应完毕后将样品取出，清洗，吹干。5) After the reaction is completed, the sample is taken out, washed, and dried.
进一步，步骤2)中所述电子束蒸发法的具体工艺条件为背景真空为5×10-4～3×10-3pa,衬底温度为25～30℃，生长速度为0.15nm/s,所用铜蒸发源的纯度为99.999wt％,所得铜薄膜的厚度为50～500nm。Further, the specific process conditions of the electron beam evaporation method in step 2) are that the background vacuum is 5×10 -4 ~ 3×10 -3 Pa, the substrate temperature is 25 ~ 30°C, and the growth rate is 0.15nm/s, The purity of the copper evaporation source used is 99.999wt%, and the thickness of the obtained copper film is 50-500nm.
进一步，步骤3)中所述前驱溶液中CuCl2的浓度为0.05～2mol/L,聚乙烯吡咯烷酮的浓度为0.1～1g/L,KI的浓度为0.05～2mol/L。Further, the concentration of CuCl 2 in the precursor solution in step 3) is 0.05-2 mol/L, the concentration of polyvinylpyrrolidone is 0.1-1 g/L, and the concentration of KI is 0.05-2 mol/L.
进一步，步骤4)中水热反应的时间为30～180min。Further, the hydrothermal reaction time in step 4) is 30-180 min.
本发明的有益效果是：The beneficial effects of the present invention are:
1)本发明首次利用Cu薄膜和水热合成蒸发出的碘蒸气作为反应原材料，在低温高压条件下制备出大面积均匀的CuI纳米材料，制备工艺与光电器件制备工艺兼容；1) For the first time, the present invention uses Cu thin film and iodine vapor evaporated by hydrothermal synthesis as reaction raw materials to prepare large-area and uniform CuI nanomaterials under low temperature and high pressure conditions, and the preparation process is compatible with the preparation process of optoelectronic devices;
2)本方法制备的CuI纳米结构大面积均匀、致密，结晶质量高且具有优异的光电性能，满足其在光电器件领域中的应用；2) The CuI nanostructure prepared by the method is uniform and dense in a large area, has high crystal quality and has excellent photoelectric performance, which satisfies its application in the field of photoelectric devices;
3)本发明的制备方法简单、反应温度低、反应时间短，成本低廉，制备条件均处于密闭空间内，减少了碘对环境的污染，是一种环境友好型制备方法，适合于大规模工业化生产。3) The preparation method of the present invention is simple, the reaction temperature is low, the reaction time is short, the cost is low, and the preparation conditions are all in a closed space, which reduces the pollution of iodine to the environment. It is an environmentally friendly preparation method and is suitable for large-scale industrialization Production.
附图说明Description of drawings
图1为本发明水热反应装置内部结构示意图；Fig. 1 is a schematic diagram of the internal structure of the hydrothermal reaction device of the present invention;
图2为本发明实施例1所得CuI纳米结构的SEM图；Fig. 2 is the SEM picture of CuI nanostructure obtained in Example 1 of the present invention;
图3为本发明实施例1所得CuI纳米结构的XRD图；Fig. 3 is the XRD pattern of CuI nanostructure obtained in Example 1 of the present invention;
图4为本发明实施例1所得CuI纳米结构的光致发光谱图；Fig. 4 is the photoluminescence spectrogram of CuI nanostructure obtained in Example 1 of the present invention;
具体实施方式detailed description
以下结合实例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。The principles and features of the present invention are described below in conjunction with examples, which are only used to explain the present invention and are not intended to limit the scope of the present invention.
实施例1：Example 1:
一种CuI纳米结构的制备方法，包括如下步骤：A method for preparing a CuI nanostructure, comprising the steps of:
1)单晶硅(100)基片进行标准的RCA清洗，去除表面的有机物、金属离子杂质及灰尘，氮气吹干后装入电子束蒸发装置的真空生长室；1) The monocrystalline silicon (100) substrate is cleaned by standard RCA to remove organic matter, metal ion impurities and dust on the surface, blown dry with nitrogen gas, and put it into the vacuum growth chamber of the electron beam evaporation device;
2)电子束蒸发法在单晶硅(100)基片的表面生长一层铜薄膜，其具体工艺条件为背景真空为5×10-4～3×10-3pa,衬底温度为25～30℃，生长速度为0.15nm/s,所用铜蒸发源的纯度为99.999wt％,所得铜薄膜的厚度为200nm；2) Electron beam evaporation method grows a layer of copper thin film on the surface of single crystal silicon (100) substrate. The specific process conditions are that the background vacuum is 5×10 -4 ~ 3×10 -3 Pa, and the substrate temperature is 25 ~ 30°C, the growth rate is 0.15nm/s, the purity of the copper evaporation source used is 99.999wt%, and the thickness of the obtained copper film is 200nm;
3)将步骤2)所得硅基铜薄膜如图1所示悬挂于反应釜中，反应釜的前驱体溶液中CuCl2的浓度为0.1mol/L,聚乙烯吡咯烷酮的浓度为0.5g/L,KI的浓度为1mol/L，充分混合搅拌，反应釜中溶液的总量约占反应釜体积的2/3；3) Hang the silicon-based copper film obtained in step 2) in the reactor as shown in Figure 1 , the concentration of CuCl in the precursor solution of the reactor is 0.1mol/L, and the concentration of polyvinylpyrrolidone is 0.5g/L, The concentration of KI is 1mol/L, fully mixed and stirred, the total amount of solution in the reactor accounts for about 2/3 of the volume of the reactor;
4)将反应釜密封后置于鼓风干燥箱内，于160℃条件下水热反应120min；4) Seal the reaction kettle and place it in a blast drying oven, and conduct a hydrothermal reaction at 160°C for 120 minutes;
5)反应完毕后将样品取出，去离子水清洗，氮气吹干。5) After the reaction, the sample was taken out, washed with deionized water, and dried with nitrogen.
实施例2：Example 2:
一种CuI纳米结构的制备方法，包括如下步骤：A method for preparing a CuI nanostructure, comprising the steps of:
1)单晶硅(100)基片进行标准的RCA清洗，去除表面的有机物、金属离子杂质及灰尘，氮气吹干后装入电子束蒸发装置的真空生长室；1) The monocrystalline silicon (100) substrate is cleaned by standard RCA to remove organic matter, metal ion impurities and dust on the surface, blown dry with nitrogen gas, and put it into the vacuum growth chamber of the electron beam evaporation device;
2)电子束蒸发法在单晶硅(100)基片的表面生长一层铜薄膜，其具体工艺条件为背景真空为5×10-4～3×10-3pa,衬底温度为25～30℃，生长速度为0.15nm/s,所用铜蒸发源的纯度为99.999wt％,所得铜薄膜的厚度为50nm；2) Electron beam evaporation method grows a layer of copper thin film on the surface of single crystal silicon (100) substrate. The specific process conditions are that the background vacuum is 5×10 -4 ~ 3×10 -3 Pa, and the substrate temperature is 25 ~ 30°C, the growth rate is 0.15nm/s, the purity of the copper evaporation source used is 99.999wt%, and the thickness of the obtained copper film is 50nm;
3)将步骤2)所得硅基铜薄膜如图1所示悬挂于反应釜中，反应釜的前驱体溶液中CuCl2的浓度为0.05mol/L,聚乙烯吡咯烷酮的浓度为0.1g/L,KI的浓度为0.05mol/L，充分混合搅拌，反应釜中溶液的总量约占反应釜体积的2/3；3) Hang the silicon-based copper film obtained in step 2) in the reactor as shown in Figure 1 , the concentration of CuCl in the precursor solution of the reactor is 0.05mol/L, and the concentration of polyvinylpyrrolidone is 0.1g/L, The concentration of KI is 0.05mol/L, fully mixed and stirred, the total amount of solution in the reactor accounts for about 2/3 of the volume of the reactor;
4)将反应釜密封后置于鼓风干燥箱内，于120℃条件下水热反应180min；4) Seal the reaction kettle and place it in a blast drying oven, and conduct a hydrothermal reaction at 120°C for 180 minutes;
5)反应完毕后将样品取出，去离子水清洗，氮气吹干。5) After the reaction, the sample was taken out, washed with deionized water, and dried with nitrogen.
实施例3：Example 3:
一种CuI纳米结构的制备方法，包括如下步骤：A method for preparing a CuI nanostructure, comprising the steps of:
1)单晶硅(100)基片进行标准的RCA清洗，去除表面的有机物、金属离子杂质及灰尘，氮气吹干后装入电子束蒸发装置的真空生长室；1) The monocrystalline silicon (100) substrate is cleaned by standard RCA to remove organic matter, metal ion impurities and dust on the surface, blown dry with nitrogen gas, and put it into the vacuum growth chamber of the electron beam evaporation device;
2)电子束蒸发法在单晶硅(100)基片的表面生长一层铜薄膜，其具体工艺条件为背景真空为5×10-4～3×10-3pa,衬底温度为25～30℃，生长速度为0.15nm/s,所用铜蒸发源的纯度为99.999wt％,所得铜薄膜的厚度为50nm；2) Electron beam evaporation method grows a layer of copper thin film on the surface of single crystal silicon (100) substrate. The specific process conditions are that the background vacuum is 5×10 -4 ~ 3×10 -3 Pa, and the substrate temperature is 25 ~ 30°C, the growth rate is 0.15nm/s, the purity of the copper evaporation source used is 99.999wt%, and the thickness of the obtained copper film is 50nm;
3)将步骤2)所得硅基铜薄膜如图1所示悬挂于反应釜中，反应釜的前驱体溶液中CuCl2的浓度为2mol/L,聚乙烯吡咯烷酮的浓度为1g/L,KI的浓度为2mol/L，充分混合搅拌，反应釜中溶液的总量约占反应釜体积的2/3；3) Hang the silicon-based copper film obtained in step 2) in the reactor as shown in Figure 1 , the concentration of CuCl in the precursor solution of the reactor is 2mol/L, the concentration of polyvinylpyrrolidone is 1g/L, and the concentration of KI The concentration is 2mol/L, fully mixed and stirred, the total amount of solution in the reactor accounts for about 2/3 of the volume of the reactor;
4)将反应釜密封后置于鼓风干燥箱内，于200℃条件下水热反应30min；4) Seal the reaction kettle and place it in a blast drying oven, and conduct a hydrothermal reaction at 200°C for 30 minutes;
5)反应完毕后将样品取出，去离子水清洗，氮气吹干。5) After the reaction, the sample was taken out, washed with deionized water, and dried with nitrogen.
为了验证本发明提供的制备方法的有益效果，我们对实施例1所得的CuI纳米结构进行了表征，如图2～4所示，从图2中可以看出，我们所制备的样品具有均匀致密的片状结构。利用X射线衍射仪表征了CuI纳米结构的结晶质量，从图3中可以看到，所制备的样品呈现多晶结构，其中220方向为CuI的优先生长方向。利用325nm的激光作为激发光源测试了CuI纳米结 构的光致发光光谱，从图4中可以发现，CuI的光致发光光谱由410nm的带边发射以及和碘空位缺陷相关的宽带光谱(600～800nm)组成。In order to verify the beneficial effect of the preparation method provided by the present invention, we characterized the CuI nanostructure obtained in Example 1, as shown in Figures 2 to 4, as can be seen from Figure 2, our prepared samples have uniform and dense flaky structure. The crystalline quality of the CuI nanostructure was characterized by X-ray diffractometer. It can be seen from Figure 3 that the prepared sample presents a polycrystalline structure, in which the 220 direction is the preferential growth direction of CuI. The photoluminescence spectrum of the CuI nanostructure was tested using a 325nm laser as the excitation light source. It can be found from Figure 4 that the photoluminescence spectrum of CuI consists of a band-edge emission at 410nm and a broadband spectrum (600-800nm) related to iodine vacancy defects. )composition.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within range.
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| CN108677155A (en) * | 2018-05-23 | 2018-10-19 | 哈尔滨工业大学 | A method of preparing cuprous iodide p-type transparent semiconductor film material at room temperature |
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| CN113699505A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院微电子研究所 | Preparation method of doped cuprous iodide film |
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| CN113699505B (en) * | 2020-05-20 | 2022-08-30 | 中国科学院微电子研究所 | Preparation method of doped cuprous iodide film |
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