CN114717000A - Colloidal silicon nanocrystal with high fluorescence quantum yield and preparation method and application thereof - Google Patents

Colloidal silicon nanocrystal with high fluorescence quantum yield and preparation method and application thereof Download PDF

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CN114717000A
CN114717000A CN202210107253.3A CN202210107253A CN114717000A CN 114717000 A CN114717000 A CN 114717000A CN 202210107253 A CN202210107253 A CN 202210107253A CN 114717000 A CN114717000 A CN 114717000A
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ncs
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colloidal silicon
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fluorescence quantum
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郝惠莲
赵悦
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Shanghai University of Engineering Science
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    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
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Abstract

The invention relates to the field of preparation technology of functional nano materials and application of the functional nano materials in photoelectric devices, in particular to preparation of colloidal silicon nanocrystals (c-Si NCs) with high fluorescence quantum yield and application of the colloidal silicon nanocrystals to OLEDs. The method mainly uses bulk monocrystalline silicon wafers, organic solvents and hydrofluoric acid (HF) solutions to be mixed, c-SiNCs with high fluorescence quantum efficiency, good surface functionalization and uniform dispersion are generated in one step through femtosecond laser liquid phase ablation, the used consumable material is low in cost, the used reagents are non-toxic and free of strong corrosivity, and the prepared c-Si NCs have the characteristics of being non-toxic, high in fluorescence quantum efficiency (up to 78.5%), easy in size distribution, easy in light-emitting wavelength regulation and the like. The c-Si NCs film is prepared from the prepared c-Si NCs solution by adopting a one-step spin coating method and is applied to an OLED, and the external quantum efficiency can be up to 7.2%. The process does not need complex chemical modification, is simple and easy to implement, has good repeatability, has good stability in an amplification experiment, and has wide industrial application prospect.

Description

Colloidal silicon nanocrystal with high fluorescence quantum yield and preparation method and application thereof
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to colloidal silicon nanocrystals with high fluorescence quantum yield, a preparation method thereof and application thereof in producing OLED (organic light emitting diode).
Background
The Bohr radius of the silicon nanocrystals (Si NCs) is less than 5.0nm, and the quantum structure of the silicon nanocrystals has a strong quantum confinement effect. Meanwhile, silicon has the advantages of high content, no toxicity, environmental friendliness and the like in the earth crust, and is applied to the fields of photoelectric devices and biological detectors more and more in recent years. Colloidal silicon nanocrystals (c-Si NCs) have the advantages of good solution dispersibility, luminescence stability and easy solution processing, and thus, in recent years, new semiconductor nanodevices based on non-traditional processes, such as light emitting diodes [ s.y.zhao, et al.ieee Transactions on Electron Devices 2018,65, 577-. Meanwhile, the colloidal silicon quantum dot has the advantages of environmental friendliness, biocompatibility and good fluorescence performance, and is widely applied to the field of novel low-cost and environment-friendly quantum dot devices at present.
Commonly used ligands for surface functionalization of c-Si NCs are hydrides [ Hanrahan M P, et al. chem. Mater.2017, 2910339-51 ] and halides [ Yuan Z, et al. nanoscale 2016, 91193-200 ], but Si NCs surfaces constructed with the ligands are susceptible to oxidation, which reduces photoluminescence quantum efficiency (PL QY). Experiments show that the Si NCs solution passivated by the alkyl has good stability and dispersivity. The commonly used methods for preparing alkyl passivated c-Si NCs are plasma enhanced chemical vapor deposition, hydrosilylation, wet chemical synthesis and the like, but the preparation methods need two or more steps, the process is complicated, and more toxic byproducts are generated.
The method for preparing the c-Si NCs commonly used in recent years is a laser liquid phase ablation technology, and has the advantages of one-step synthesis, simple and feasible process, easy regulation and control of laser parameters and the like. However, laser ablation techniques tend to cause surface oxidation of Si NCs, resulting in PL degradation, limiting their application in optoelectronic devices and bio-detection.
Therefore, in order to overcome the defects of the existing technology for preparing c-Si NCs, such as surface oxidation and low photoluminescence quantum efficiency, the preparation process needs to be improved to obtain c-Si NCs with stable performance, narrow size distribution, adjustable size and luminescence wavelength and high photoluminescence efficiency.
Disclosure of Invention
The invention aims to solve the technical problems that the existing technology for preparing c-Si NCs is easy to cause the defects of surface oxidation, low photoluminescence quantum efficiency and the like, and provides a method for preparing the c-Si NCs with stable performance, narrow size distribution, adjustable size and luminescence wavelength and high photoluminescence efficiency by adding HF solution as a ligand in an organic solvent.
The technical problem to be solved by the invention is to provide a preparation method of the c-Si NCs solution.
The invention finally solves the technical problem of providing the application of the c-Si NCs solution on the OLED.
In order to solve the problems in the prior art, the invention discloses a preparation method of colloidal silicon nanocrystals (c-Si NCs), which comprises the following steps:
(1) completely immersing the cleaned and dried monocrystalline silicon wafer into a mixed solution of an organic solvent and an HF solution;
(2) stirring and ablating with femtosecond laser;
(3) and centrifuging the mixed solution subjected to the femtosecond laser ablation treatment, and taking the upper colloidal solution.
Preferably, the monocrystalline silicon wafer in step (1) is p-type and has a thickness of about 350 μm;
the organic solvent in the step (1) is toluene; in the mixed solution, the volume percentage of the HF solution is 0-15%, preferably 0.1-15%, and more preferably 5-10%; in a preferred embodiment of the present invention, the volume percentage of the HF solution in the mixed solution is 10%; the concentration of the HF solution is 45 wt% -55 wt%, preferably 50 wt%.
In the mixed system, the concentration of HF is 0-95g/L, preferably 0.5-90 g/L; more preferably 25 to 90 g/L.
In a preferred embodiment of the present invention, the HF content in the mixed system is 55 to 60 g/L.
The stirring in the step (2) is magnetic stirring.
In the step (2), the laser femtosecond laser process parameters are as follows: wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm-2；
In the step (2), the femtosecond laser ablation time is 60 min;
the centrifugal treatment conditions in the step (3) are as follows: the centrifugal speed is 15000 rpm; the centrifugation times are 3 times; the centrifugation time was 30min each time.
A colloidal silicon nanocrystal having a high fluorescence quantum yield can be obtained by the above method. Has the characteristics of stable optical performance, narrow size distribution and adjustable and controllable light-emitting wavelength and intensity.
The c-Si NCs prepared by the above method are made into thin films (for example, by spin coating) and can be used for preparing OLED (organic light emitting semiconductor).
An OLED contains the colloidal silicon nanocrystals.
The invention has the advantages that compared with the prior art, the invention has the following advantages:
the method takes the monocrystalline silicon piece as the raw material to prepare the c-Si NCs solution, and the raw material has low cost and is nontoxic; and the femtosecond laser liquid phase ablation technology is used in the preparation process, so that Si NCs can be prepared in one step.
The process of the invention adopts toluene as solvent, and because of the regular pentacyclic structure, when the silicon nano-crystalline particles react with monocrystalline silicon at high temperature under laser ablation, the silicon nano-crystalline particles with uniform size, good dispersion and complete surface modification can be effectively generated; the HF used in the mixed solvent can effectively passivate oxygen defects on the surface of the silicon nanocrystal, so that the structure and the optical stability of the silicon nanocrystal are improved, and the fluorescence quantum efficiency of the silicon nanocrystal is improved.
In order to further solve the problem that PL QY is low due to the fact that the surface of Si NCs is oxidized in the laser ablation process, the invention uses an organic solvent and HF mixed solution as a ligand, and the addition of the HF solution can effectively passivate oxygen dangling bonds generated by the oxidation of the surface of the Si NCs in the ablation process, so that the luminescence and PL QY of the c-Si NCs are effectively improved, and the colloidal silicon nanocrystal which is stable in performance, narrow in size distribution, adjustable in size and luminescence wavelength and high in photoluminescence efficiency is obtained.
In the whole preparation process, a large amount of strong corrosive or toxic chemical raw materials such as acid and alkali are not needed to be consumed, and the preparation method is non-toxic and harmless to the environment; the process is simple and easy to implement, does not need complex chemical modification, is easy to regulate and control process parameters, has good repeatability in the preparation process, has good stability in an amplification experiment, and has wide industrial application prospect.
The c-Si NCs obtained by the method have the characteristics of no toxicity, no harm, high fluorescence quantum efficiency (up to 78.5%), easy size distribution, easy regulation and control of luminescence wavelength and the like. Can be widely applied to the fields of photoelectric devices such as LED, solar photovoltaic, biological fluorescent mark and the like. The c-Si NCs film is prepared from the prepared c-Si NCs solution by adopting a one-step spin coating method and is applied to the OLED, and the external quantum efficiency can reach 7.2%.
Drawings
FIG. 1 is a TEM photograph of colloidal silicon nanocrystals prepared in example 3.
Fig. 2 is a size distribution diagram of colloidal silicon nanocrystals prepared in example 3.
Fig. 3 is a fourier transform infrared spectrum of the colloidal silicon nanocrystal prepared in example 3.
Fig. 4 is a graph of the uv-vis absorption spectrum of the colloidal silicon nanocrystal prepared in example 3.
FIG. 5 is a fluorescence emission spectrum of colloidal silicon nanocrystals prepared in example 3 under excitation of different excitation wavelengths.
FIG. 6 is a transmission electron micrograph and a size distribution chart of c-Si NCs prepared under the conditions of examples 1 to 4, wherein (a), (c), (e) and (f) are transmission electron micrographs of c-Si NCs prepared under the conditions of examples 1 to 4, and (b), (d), (f) and (h) are size distribution charts corresponding to c-Si NCs prepared under the conditions of examples 1 to 4.
FIG. 7 is a photoluminescence image of Si NCs prepared under the conditions of examples 1 to 4, wherein the excitation wavelength is 325 nm. The curves are, from top to bottom, examples 3,1, 2 and 4.
Detailed Description
In order to better understand the invention, the technical scheme of the invention is further detailed and completely described in the following by combining specific experimental implementation and detailed proportion.
Example 1
(1) A1 cm × 1cm monocrystalline silicon wafer (thickness-350 μm, p-type (100)) cleaned and dried by alcohol, deionized water and the like is placed in a sample bottle, 15ml of toluene (> 99%) solution is added, a magnetic stirrer is placed, and the sample bottle is placed on the magnetic stirrer.
(2) While magnetically stirring, passing through a titanium/sapphire laser (wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm)-2) Liquid phase ablation for 60 min.
(3) Centrifuging the ablated sample at a high speed of 15000rpm for 3 times, wherein the time duration of each time is 30 min; the upper solution obtained by separation was slightly cloudy.
The PL QY of the c-Si NCs obtained in example 1 was 48.6% according to the above formula.
The obtained upper layer solution is respectively subjected to structural characterization such as XRD, XPS, FTIR, HRTEM and the like, and optical properties such as PL, time-resolved PL and ultraviolet absorption spectrum (UV-vis absorbance spectrum) are characterized. The following examples follow the same characterization method.
Example 2
(1) A1 cm X1 cm piece of the same single crystal silicon as in example 1 was taken, placed in a sample bottle, 15ml of a mixed solvent of toluene (> 99%) and HF solution was added, and placed on a magnetic stirrer. The purity of the toluene used in the mixed solution is > 99%; the HF solution was added in a concentration of 50 wt% (specific gravity 1.157), 5.0% by volume in the mixed solution, and the HF content was about 28 to 30 g/L.
(2) While magnetically stirring, passing through titanium/sapphire femtosecond laser (wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm)-2) Liquid phase ablation for 60 min.
(3) Centrifuging the ablated sample at a high speed of 15000rpm for 3 times, wherein the time duration of each time is 30 min; the upper clear liquid was isolated as a pale yellow color.
The PL QY of the obtained c-Si NCs was 65.7%.
Example 3
(1) A1 cm X1 cm piece of the same single crystal silicon as in example 1 was taken, placed in a sample bottle, 15ml of a mixed solvent of toluene (> 99%) and HF solution was added, and placed on a magnetic stirrer. The purity of the toluene used in the mixed solution is > 99%; the concentration of the added HF solution was 50 wt%, the volume percentage in the mixed solution was 10.0%, and the HF content was about 57-59 g/L.
(2) While magnetically stirring, passing through titanium/sapphire femtosecond laser (wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm)-2) Liquid phase ablation for 60 min.
(3) Centrifuging the ablated sample at a high speed of 15000rpm for 3 times, wherein the time duration of each time is 30 min; the upper clear liquid was isolated as a pale yellow color.
PL QY of the obtained c-Si NCs was 77.2%.
Fig. 1 is a transmission electron microscope image of the colloidal silicon nanocrystals prepared in example 3, which shows that the prepared c-Si NCs are spherical particles with uniform distribution, and have good monodispersity and uniform size, and the particle size is-3.0 nm, and the insert in the upper right corner shows a high-resolution transmission electron microscope image, which shows that the Si NCs have uniform lattice planes, the lattice spacing is about 0.31nm, and the insert in the upper left corner shows an electron selection diffraction image of the prepared c-Si NCs, and the regular circles show that the prepared Si NCs have good crystallinity.
FIG. 2 is a graph showing the size distribution of c-Si NCs prepared in example 3, and it can be seen that the size of Si NCs is about 3.0nm and the size distribution is narrow.
FIG. 3 is a Fourier infrared absorption spectrum of c-Si NCs prepared in example 3, showing a spectrum at 670cm-1The Si-C bond of (2) and the absence of an oxygen dangling bond indicate that Si NCs have a good surface structure.
FIG. 4 is an ultraviolet-visible absorption spectrum of c-Si NCs prepared in example 3, which shows that Si NCs have a strong absorption in the ultraviolet-visible region (200-650 nm) and a large absorption peak at 366 nm.
FIG. 5 is a room temperature photoluminescence spectrum of c-Si NCs prepared in example 3 at different excitation light wavelengths. Under different excitation wavelengths in the wavelength range of 330-370 nm, the photoluminescence wavelength of the c-Si NCs is almost independent of the excitation light. The fluorescence intensity is maximal at an excitation wavelength of 360 nm.
The colloidal silicon nanocrystalline solution prepared in the embodiment 3 is used for preparing a colloidal silicon nanocrystalline film by adopting a one-step spin coating method and is applied to an OLED (organic light emitting diode), and the external quantum efficiency can be up to 7.2% through detection.
Example 4
(1) A1 cm X1 cm piece of the same single crystal silicon as in example 1 was taken, placed in a sample bottle, 15ml of a mixed solvent of toluene (> 99%) and HF solution was added, and placed on a magnetic stirrer. The purity of the toluene used in the mixed solution is > 99%; the concentration of the added HF solution was 50 wt%, the volume percentage in the mixed solution was 15.0%, and the HF content was about 85-88 g/L.
(2) While magnetically stirring, passing through titanium/sapphire femtosecond laser (wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm)-2) Liquid phase ablation for 60 min.
(3) Centrifuging the ablated sample at a high speed of 15000rpm for 3 times, wherein the time duration of each time is 30 min; the upper clear liquid was isolated as a pale yellow color.
The PL QY of the obtained c-Si NCs was 68.4%.
FIG. 6 is a transmission electron micrograph and a size distribution chart of c-Si NCs prepared under the conditions of examples 1 to 4, wherein (a), (c), (e) and (f) are transmission electron micrographs of c-Si NCs prepared under the conditions of examples 1 to 4, and (b), (d), (f) and (h) are size distribution charts corresponding to c-Si NCs prepared under the conditions of examples 1 to 4. It can be seen from the figure that the particle size varies with the laser ablation time and the amount of HF solution added.
FIG. 7 is a photoluminescence image of Si NCs prepared under the conditions of examples 1 to 4, wherein the excitation wavelength is 325 nm. The curves are, from top to bottom, examples 3,1, 2 and 4. It can be seen from the figure that the photoluminescence intensity of example 3 is significantly higher than that of the Si NCs in the other examples.
In summary, we chose example 3 as the preferred option.
The invention provides a colloidal silicon nanocrystal solution with high photoluminescence efficiency, a preparation method thereof and a thought and a method for feasible application. There are many ways and ways to implement this solution, and the above description is only a preferred embodiment of the present invention.

Claims (9)

1. A method for preparing colloidal silicon nanocrystals with high fluorescence quantum yield is characterized by comprising the following steps:
(1) completely immersing the cleaned and dried monocrystalline silicon wafer into a mixed solution of an organic solvent and an HF solution;
(2) stirring and ablating by femtosecond laser;
(3) and centrifuging the mixed solution subjected to the femtosecond laser ablation treatment, and taking the upper colloidal solution.
2. The method as claimed in claim 1, wherein the single-crystal silicon wafer in step (1) is p-type with a thickness of 300-400 μm.
3. The process according to claim 1, wherein the organic solvent in the step (1) is toluene; in the mixed solution, the volume percentage of the HF solution is 0-15%, and the concentration of the HF solution is 45-55 wt%.
4. The method according to claim 1, wherein the volume of the HF solution in the step (1) is 0.1% to 15%.
5. The preparation method according to claim 1, wherein in the step (2), the laser femtosecond laser process parameters are as follows: wavelength 800nm, pulse width 100fs, frequency 80MHz, laser energy density 0.2mJ cm-2And the femtosecond laser ablation time is 60 min.
6. The method according to claim 1, wherein in the step (3), the centrifugal treatment conditions are as follows: the centrifugation speed is 15000rpm, the centrifugation times are 3 times, and the centrifugation time is 30min each time.
7. Colloidal silicon nanocrystals with high fluorescence quantum yield, obtained by the preparation process according to any one of claims 1 to 6.
8. Use of colloidal silicon nanocrystals according to claim 8 for the preparation of OLEDs.
9. An OLED comprising the colloidal silicon nanocrystal of claim 8.
CN202210107253.3A 2022-01-28 2022-01-28 Colloidal silicon nanocrystal with high fluorescence quantum yield and preparation method and application thereof Pending CN114717000A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107057691A (en) * 2017-06-19 2017-08-18 上海工程技术大学 A kind of preparation method of the colloidal state silicon nanocrystal of surface modification

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107057691A (en) * 2017-06-19 2017-08-18 上海工程技术大学 A kind of preparation method of the colloidal state silicon nanocrystal of surface modification

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* Cited by examiner, † Cited by third party
Title
张迎兄: ""胶体硅量子点的制备及其表面改性的研究"" *
曹小龙,李清山,张淑芳: "硅纳米颗粒和多孔硅的荧光光谱研究" *

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