Large-area nanoparticle array and preparation method thereof

Abstract

The invention provides a large-area nanoparticle array and a preparation process thereof. The preparation method of the large-area nano-particle array comprises the step of directly depositing and preparing the nano-particle array on glass, silicon or other substrates through a one-step method by adopting magnetron sputtering or other physical vapor deposition equipment. The preparation method is low in cost, stable and mature industrial magnetron sputtering equipment can be used, the nano-particle array can be directly deposited and prepared on other substrates such as large-area glass, silicon wafers and ceramics through a one-step method, and the preparation method has the advantage of large-scale production. The prepared large-area nanoparticle array can be used in the fields of solar cells, surface enhanced Raman, photoetching, reactive ion etching, nanoimprinting and the like, and has great economic value.

Description

Technical Field

[0001] The invention belongs to the technical field of nanoparticle array and nanostructure preparation, and specifically relates to a large-area nanoparticle array and a preparation method thereof. Background Art

[0002] Large-area nanoparticle arrays have a wide range of application scenarios in the fields of chips, solar cells, surface-enhanced Raman, etc. Chips are one of the main application scenarios of high-tech nanotechnology. As the requirements for power consumption and performance increase, higher requirements are also put forward for nanotechnology. Solar cells invest billions of dollars in battery electrical performance each year, but their efficiency improvement does not exceed 0.5% each year. Therefore, improving its light absorption and thus improving efficiency from an optical point of view is a different approach, which is expected to greatly improve device efficiency. Surface-enhanced Raman has higher and higher requirements for detection accuracy, and the requirements for surface nanoparticle arrays are also rising. Conventional preparation methods for nanoparticle arrays, such as the sol-gel method, the single film layer method, and the method of thin film deposition followed by annealing, are usually difficult to prepare large-area nanoparticle arrays, or the preparation method has a high cost. The present invention proposes a simple one-step method for directly depositing and preparing large-area nanoparticle arrays. Summary of the invention

[0003] The purpose of the present invention is to provide a large-area nanoparticle array and a preparation method thereof. By adopting the technical scheme of the present invention, a large-area nanoparticle array can be prepared, and the preparation method is simple, which is convenient for large-scale promotion and use.

[0004] To achieve the above-mentioned object of the invention, the technical solution of the present invention is as follows: The present invention provides a method for preparing large-area nanoparticles, that is, using magnetron sputtering or other physical vapor deposition equipment to directly deposit and prepare nanoparticle arrays on glass, silicon or other substrates in one step.

[0005] Furthermore, the preparation method of the large-area nanoparticle array is characterized in that the physical vapor deposition method is mainly magnetron sputtering and thermal evaporation.

[0006] Furthermore, the method for preparing the large-area nanoparticle array is characterized in that the substrate can be glass, silicon, or ceramic.

[0007] Furthermore, the method for preparing the large-area nanoparticle array is characterized in that the raw materials used for the magnetron sputtering target or thermal evaporation are metal silver, molybdenum, nickel, gold, titanium, vanadium, and tungsten.

[0008] Furthermore, the method for preparing the large-area nanoparticle array is characterized in that the physical vapor deposition rate is controlled to be less than 200nm / min. The power density of the magnetron sputtering on the target should be less than 10W / cm 2 .

[0009] Furthermore, the preparation method of the large-area nanoparticle array is characterized in that the physical vapor deposition deposition needs to be completed within 20 minutes. Furthermore, the method for preparing the large-area nanoparticle array is characterized in that a reactive gas such as oxygen can be introduced during the physical vapor deposition process to generate a nanoparticle array with oxides.

[0010] Furthermore, when the deposition method is magnetron sputtering, the typical settings are: DC sputtering of a water-cooled silver target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar, the working pressure is 1.6 Pa, the argon flow rate is 30 sccm, the sputtering voltage is about 225 V, the current is about 0.01 A, and the deposition time is 10 s. Its power density is estimated to be about 0.2 W / cm 2 .

[0011] Furthermore, the preparation method of the large-area nanoparticle array is characterized in that the prepared large-area nanoparticle array can be used on the absorption layer of a solar cell to produce plasma polarization effect, localized plasma resonance effect, scattering effect, etc., thereby enhancing light absorption; the prepared large-area nanoparticle array can also be used as a mask for photolithography, reactive ion etching, nanoimprinting, etc.; it can also be used for surface enhanced Raman.

[0012] Furthermore, the nanoparticle array prepared by any of the preparation methods described above and its application. Compared with the prior art, the advantages and beneficial effects of the present invention are: The present invention adopts physical vapor deposition, mainly magnetron sputtering, to directly deposit and prepare a large-area nanoparticle array in one step. The process is simple, the deposition time is usually short, and it is conducive to large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 1.

[0014] Figure 2 is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 2.

[0015] Figure 3 This is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 3. The corresponding sputtering voltage is 280 V and the current is 0.04 A.

[0016] Figure 4 This is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 3. The corresponding sputtering voltage is 272 V and the current is 0.03 A.

[0017] Figure 5 This is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 3. The corresponding sputtering voltage is 259 V and the current is 0.02 A.

[0018] Figure 6 is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 4.

[0019] Figure 7 is a typical scanning electron microscope (SEM) photograph of the nanoparticle array prepared in Example 5. Implementation

[0020] The following embodiments are used to better illustrate the present invention, but the present invention is not limited to the following embodiments.

[0021] Example 1: Preparation of silver nanoparticle arrays Nanoparticle arrays were prepared on glass using magnetron sputtering silver targets. The specific steps are as follows: Preparation of silver nanoparticle arrays by direct deposition using magnetron sputtering: Back vacuum is 10 -4 Pa level, DC sputtering of a water-cooled Ag target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar (99.9995%), the working gas pressure is 1.6 Pa; the argon gas flow rate is 30 sccm, the sputtering voltage is about 225 V, the current is about 0.01 A, and the deposition time is 10 s.

[0022] The nanoparticle array prepared in Example 1 was observed by scanning electron microscope (SEM). Figure 1 As shown in the figure (the particles are silver nanoparticles), the results show that nanoparticles were successfully prepared. Nanoparticles of about 10nm are dispersed and evenly distributed. This structure is suitable for photolithography, reactive ion etching, surface enhanced Raman, etc. Example

[0023] Nanoparticle arrays were prepared on polished silicon wafers using magnetron sputtering of silver targets. The specific steps are as follows: Preparation of silver nanoparticle arrays by direct deposition using magnetron sputtering: Back vacuum is 10 -4 Pa level, DC sputtering of a water-cooled Ag target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar (99.9995%), the working gas pressure is 1.6 Pa; the argon gas flow rate is 30 sccm, the sputtering voltage is about 225 V, the current is about 0.01 A, and the deposition time is 10 s.

[0024] The nanoparticle array prepared in Example 2 was observed by scanning electron microscope (SEM). Figure 2As shown in the figure (the particles are silver nanoparticles), the results show that nanoparticles were successfully prepared. Nanoparticles of about 20nm are dispersed and evenly distributed. This structure is suitable for use in solar cells to exert its plasma effect, as well as lithography, reactive ion etching, nanoimprinting, and surface enhanced Raman. Example

[0025] Nanoparticle arrays were prepared on glass using magnetron sputtering silver targets. The specific steps are as follows: Preparation of silver nanoparticle arrays by direct deposition using magnetron sputtering: Back vacuum is 10 -4 Pa level, DC sputtering of a water-cooled Ag target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar (99.9995%), the working gas pressure is 1.6 Pa; the argon gas flow rate is 30 sccm, and the sputtering voltage and current are compared in three groups: voltage 280 V, current 0.04 A, voltage 272 V, current 0.03 A, voltage 259 V, current 0.02 A; the deposition time is 15 s.

[0026] The nanoparticle array prepared in Example 3 was observed by scanning electron microscope (SEM). Figure 3-5 As shown in the figure (the particles in the figure are silver nanoparticles), the results show that nanoparticles were successfully prepared. It can be seen that as the power decreases, the size distribution of nanoparticles becomes more and more uniform. High power can easily obtain a denser nanoparticle array with a larger size distribution range. These high-power nanoparticle arrays are more suitable for applications in solar cells and surface-enhanced Raman. Example

[0027] The nanoparticle array was prepared on glass using a nickel target by magnetron sputtering. The specific steps are as follows: Preparation of nickel nanoparticle arrays by direct deposition using magnetron sputtering: Back vacuum is 10 -4 Pa level, DC sputtering of a water-cooled nickel target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar (99.9995%), the working gas pressure is 1.6 Pa; the argon flow rate is 30 sccm, the sputtering voltage is about 265 V, the current is about 0.015 A, and the deposition time is 40 s.

[0028] The nanoparticle array prepared in Example 4 was observed by scanning electron microscope (SEM). Figure 6 As shown in the figure (the particles in the figure are nickel nanoparticles), the results show that nanoparticles were successfully prepared. Nanoparticles of about 10nm are sparsely distributed. The process parameters still need to be further optimized. Example

[0029] Nanoparticle arrays were prepared on glass using magnetron sputtering of molybdenum targets. The specific steps are as follows: Preparation of nano-molybdenum particle arrays by direct deposition using magnetron sputtering: the back vacuum is 10 -4 Pa level, DC sputtering of a water-cooled molybdenum target (99.995%) with a diameter of 60 mm, the sputtering gas is pure Ar (99.9995%), the working gas pressure is 1.6 Pa; the argon gas flow rate is 30 sccm, the sputtering voltage is about 290 V, the current is about 0.02 A, and the deposition time is 15 s.

[0030] The nanoparticle array prepared in Example 5 was observed by scanning electron microscope (SEM). Figure 7 As shown in the figure (the particles in the figure are molybdenum nanoparticles), the results show that nanoparticles were successfully prepared. The size of the nanoparticles ranges from 10nm to 100nm, and the main body is small particles. This nanoparticle array is more suitable for applications in solar cells and surface enhanced Raman. The above embodiments illustrate that the deposition rate can be adjusted by adjusting the power, gas pressure, argon gas flow rate, etc. in the magnetron sputtering film deposition process; and the deposition time can be controlled to avoid forming a continuous film. By controlling the above parameters, a nanoparticle array with controllable shape, size, and distribution can be obtained.

[0031] In addition, the prepared large-area nanoparticle arrays can be used in solar cells, surface enhanced Raman, lithography, reactive ion etching, nanoimprinting and other fields.

[0032] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for a person skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to replace some of the technical features therein by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions claimed to be protected by the present invention.

Claims

1. A method for preparing a large-area nanoparticle array, characterized in that: Nanoparticle arrays are prepared by direct deposition in one step on glass, silicon or other ceramic substrates using magnetron sputtering equipment or other physical vapor deposition equipment.

2. According to the preparation method of large-area nanoparticle arrays according to claim 1, the physical vapor deposition method is mainly magnetron sputtering and thermal evaporation.

3. According to the preparation method of large-area nanoparticle arrays described in claim 1, the substrate can be glass, silicon, or ceramic.

4. According to the preparation method of large-area nanoparticle arrays described in claim 1, the magnetron sputtering target is a metal silver, molybdenum, nickel, gold, titanium, vanadium, or tungsten target; the raw materials used for thermal evaporation are metal silver, molybdenum, nickel, gold, titanium, vanadium, or tungsten raw materials.

5. According to the method for preparing a large-area nanoparticle array according to claim 1, the physical vapor deposition rate should be controlled to be lower than 200 nm / min. Therefore, the power density of magnetron sputtering acting on the target is lower than 10 W / cm 2 . Deposition is completed in less than 20 minutes.

6. According to the method for preparing a large-area nanoparticle array according to claim 1, a reactive gas such as oxygen can be introduced during the physical vapor deposition process to generate a nanoparticle array with an oxide.

7. According to the preparation method of the large-area nanoparticle array described in claim 1, the prepared large-area nanoparticle array can be used on the absorption layer of a solar cell to produce plasma polarization effect, localized plasma resonance effect, scattering effect, etc., thereby enhancing light absorption; the prepared large-area nanoparticle array can also be used as a mask for photolithography, reactive ion etching, and nanoimprinting; it can also be used for surface enhanced Raman.

8. The nanoparticle array prepared by the preparation method according to any one of claims 1 to 7 and its application.

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