A method for preparing high-absorption tantalum nanoparticles

Abstract

The application relates to a preparation method of high-absorption tantalum nanoparticles, and belongs to the field of substrate surface nanoparticle preparation, in particular to a preparation method of high-absorption tantalum nanoparticles. The application aims at solving the technical problems of high cost and large particle size in the preparation of tantalum nanoparticles. In the application, a suitable tantalum target and a substrate are selected, the substrate is cleaned and fixed in a sputtering chamber, the vacuum degree in the sputtering chamber is adjusted, an appropriate amount of working gas is filled into the sputtering chamber, and a high-voltage electric field is applied to ionize the gas; the size, morphology and distribution of the tantalum nanoparticles are controlled by adjusting the magnetron sputtering power, sputtering time, gas pressure and other parameters. The prepared tantalum nanoparticles can effectively reduce the reflectivity, the average reflectivity can reach 9.49% in the wavelength range of 250nm-2500nm, and the average reflectivity can reach 13% in the wavelength range of 2.5mu m-25mu m.

Description

Technical Field

[0001] This invention belongs to the field of substrate surface nanoparticle preparation, specifically a method for preparing highly absorbent tantalum nanoparticles. Background Technology

[0002] Tantalum nanoparticles possess unique optical properties, such as wide-area spectral absorption and high photothermal conversion efficiency, making them potentially valuable for applications in photoacoustic imaging and photothermal therapy. Tantalum nanoparticles can also be used to prepare high-performance composite materials and coatings to improve their strength, hardness, wear resistance, and other properties.

[0003] Existing methods for preparing tantalum nanoparticles include chemical vapor deposition (CVD), vacuum plasma spraying (VPS), and plasma immersion ion implantation. However, these methods have the following problems: the dense tantalum coating films produced are difficult to obtain nanoparticles, and they require sophisticated equipment with high maintenance costs. For example, during CVD, impurities may be introduced due to gas-reactant contact and potential cross-contamination, resulting in some inhomogeneity. The uniformity and thickness distribution of the particles are difficult to control precisely, making it challenging to effectively prepare nanoparticles. Furthermore, plasma immersion ion implantation typically requires a long time to complete a single implantation process and demands significant energy to maintain plasma formation and upkeep. In summary, the cost of preparing Ta nanoparticles using existing technologies is relatively high, and the Ta nanoparticle size is relatively large.

[0004] Magnetron sputtering is a physical vapor deposition method that uses a magnetic field to control the trajectory of charged particles. During magnetron sputtering, the target material is bombarded by high-energy particles (such as argon ions), causing atoms or atomic groups on the target surface to gain enough energy to detach from the target surface and form sputtered particles. These particles are confined in a plasma region near the target material under the influence of a magnetic field, and after multiple collisions and scattering, they eventually form nanoparticles on a low surface energy surface. Summary of the Invention

[0005] The present invention aims to address the technical problems of high cost and large particle size in the current preparation of tantalum nanoparticles, and provides a method for preparing highly absorbent tantalum nanoparticles.

[0006] The method for preparing the high-absorption tantalum nanoparticles of the present invention is carried out according to the following steps:

[0007] 1. Cleaning the substrate: First, clean the substrate with high-pressure air for 5 min to 10 min, then use anhydrous ethanol for ultrasonic cleaning for 4 min to 6 min, then use ultrapure water for ultrasonic cleaning for 4 min to 6 min, blow dry with nitrogen, and modify the surface with octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate.

[0008] II. Pre-sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3 Below Pa, fix the tantalum target material, use high-purity argon as the working gas, adjust the temperature of the substrate after step one to 0-200℃, control the sputtering working vacuum at 0.8Pa-1.2Pa, the pre-sputtering power is 10W-50W, and the time is 50s-70s.

[0009] III. Secondary sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3 Below Pa, the working gas is high-purity argon. The substrate temperature is adjusted to 0-200℃, the sputtering working vacuum is controlled at 0.8Pa-1.2Pa, the sputtering power is 50W-100W, and the sputtering time is 2min-10min, so that tantalum nanoparticles are obtained on the substrate.

[0010] Compared with the prior art, the present invention has the following advantages:

[0011] I. This invention utilizes magnetron sputtering to uniformly prepare tantalum nanoparticles, and the particle size of the tantalum nanoparticles can be controlled by adjusting the process parameters.

[0012] II. The tantalum nanoparticles prepared by this invention can effectively reduce reflectivity. The average reflectivity can reach 9.49% in the wavelength range of 250nm to 2500nm and 13% in the wavelength range of 2.5μm to 25μm.

[0013] Third, the process operation of the present invention can be used for a variety of substrate materials, such as silicon wafers, quartz and ITO. Attached Figure Description

[0014] Figure 1 Infrared emissivity curves of tantalum particles prepared for experiments one through five;

[0015] Figure 2 Visible-near-infrared surface reflectance curves of tantalum particles prepared for experiments one through five. Detailed Implementation

[0016] Specific Implementation Method 1: This implementation method is a method for preparing highly absorbent tantalum nanoparticles, specifically carried out according to the following steps:

[0017] 1. Cleaning the substrate: First, clean the substrate with high-pressure air for 5 min to 10 min, then use anhydrous ethanol for ultrasonic cleaning for 4 min to 6 min, then use ultrapure water for ultrasonic cleaning for 4 min to 6 min, blow dry with nitrogen, and modify the surface with octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate.

[0018] II. Pre-sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3Below Pa, fix the tantalum target material, use high-purity argon as the working gas, adjust the temperature of the substrate after step one to 0-200℃, control the sputtering working vacuum at 0.8Pa-1.2Pa, the pre-sputtering power is 10W-50W, and the time is 50s-70s.

[0019] III. Secondary sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3 Below Pa, the working gas is high-purity argon. The substrate temperature is adjusted to 0-200℃, the sputtering working vacuum is controlled at 0.8Pa-1.2Pa, the sputtering power is 50W-100W, and the sputtering time is 2min-10min, so that tantalum nanoparticles are obtained on the substrate.

[0020] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the substrate mentioned in step one is a silicon wafer, quartz, or ITO. Everything else is the same as in Specific Implementation Method One.

[0021] Specific Implementation Method 3: This implementation method differs from Specific Implementation Method 1 or 2 in that: in step 1, the substrate is first cleaned with high-pressure air for 5 minutes, then ultrasonically cleaned with anhydrous ethanol for 4 minutes, and finally ultrasonically cleaned with ultrapure water for 4 minutes. Everything else is the same as in Specific Implementation Method 1 or 2.

[0022] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that the method for surface modification with octadecyltrichlorosilane in step one involves sonicating the substrate in a solution of octadecyltrichlorosilane. Everything else is the same as in Specific Implementation Methods One to Three.

[0023] Specific Implementation Method Five: This implementation method differs from Specific Implementation Method Four in that the temperature of the substrate after the treatment in Step One is adjusted to 25°C in Step Two. Everything else is the same as in Specific Implementation Method Four.

[0024] Specific Implementation Method Six: This implementation method differs from Specific Implementation Method Five in that the pre-sputtering power in step two is 15W and the time is 50s. Everything else is the same as in Specific Implementation Method Five.

[0025] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Method Six in that the sputtering power in step three is 50W, and the sputtering time is 2 minutes. Everything else is the same as in Specific Implementation Method Six.

[0026] The invention was verified using the following experiments:

[0027] Experiment 1: This experiment demonstrates a method for preparing highly absorbent tantalum nanoparticles, specifically carried out according to the following steps:

[0028] 1. Cleaning the substrate: First, clean the silicon substrate with high-pressure air for 5 minutes, then use anhydrous ethanol for ultrasonic cleaning for 4 minutes, then use ultrapure water for ultrasonic cleaning for 4 minutes, blow dry with nitrogen, and then sonicate the substrate in a solution of octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate.

[0029] II. Pre-sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3 Below Pa, fix the pure tantalum target material, use high-purity argon as the working gas, adjust the temperature of the substrate after step one to 25℃, control the sputtering working vacuum at 0.8Pa, the pre-sputtering power is 15W, and the time is 50s.

[0030] III. Secondary sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. -3 The working gas was high-purity argon, the substrate temperature was adjusted to 25℃, the sputtering working vacuum was controlled at 0.8Pa, the sputtering power was 50W, the sputtering time was 2min, and tantalum nanoparticles with a particle size of 50nm were obtained on the substrate.

[0031] Experiment 2: This experiment differs from Experiment 1 in that the background vacuum level of the chamber is controlled at 5 × 10⁻⁶ in step 2. -4 Below Pa, the sputtering working vacuum is controlled at 1 Pa, and the pre-sputtering power is 25 W; in step three, the chamber background vacuum is controlled at 5 × 10⁻⁶ Pa. -4 Below Pa, the sputtering working vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, and the sputtering time was 5 min. The particle size of tantalum nanoparticles obtained on the substrate was 80 nm to 100 nm. Other procedures were the same as in Experiment 1.

[0032] Experiment 3: This experiment differs from Experiment 1 in that the background vacuum level of the chamber is controlled at 5 × 10⁻⁶ in step 2. -4 Below Pa, the substrate temperature after step one is adjusted to 50℃, the sputtering working vacuum is controlled at 1 Pa, the pre-sputtering power is 25W, and the time is 70s; in step three, the chamber background vacuum is controlled at 5×10⁻⁶ Pa. -4 Below Pa, the substrate temperature was adjusted to 50℃, the sputtering working vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, and the sputtering time was 10 min. The particle size of tantalum nanoparticles obtained on the substrate was 200 nm to 300 nm. Other procedures were the same as in Experiment 1.

[0033] Experiment 4: This experiment differs from Experiment 1 in that the background vacuum level of the chamber in step 2 is controlled at 5 × 10⁻⁶. -4 Below Pa, the substrate temperature after step one is adjusted to 100℃, the sputtering working vacuum is controlled at 1 Pa, the pre-sputtering power is 25W, and the time is 20s; in step three, the chamber background vacuum is controlled at 5×10⁻⁶ Pa. -4Below Pa, the substrate temperature was adjusted to 100℃, the sputtering working vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, and the sputtering time was 15 min. The tantalum particles obtained on the substrate had a particle size of 10 μm. Other procedures were the same as in Experiment 1.

[0034] Experiment 5: This experiment differs from Experiment 1 in that the background vacuum level of the chamber in step 2 is controlled at 5 × 10⁻⁶. -4 Below Pa, the substrate temperature after step one is adjusted to 150℃, the sputtering working vacuum is controlled at 1 Pa, the pre-sputtering power is 25W, and the time is 20s; in step three, the chamber background vacuum is controlled at 5×10⁻⁶ Pa. -4 Below Pa, the substrate temperature was adjusted to 150℃, the sputtering working vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, and the sputtering time was 25 min. The tantalum particles obtained on the substrate had a particle size of 53 μm. Other procedures were the same as in Experiment 1.

[0035] Figure 1 The graph shows the infrared emissivity curves of the tantalum particles prepared for experiments one through five. The dimensions marked by the five curves in the graph are the particle sizes of the tantalum particles prepared. It can be seen that the average reflectivity of the three nanometer-sized tantalum particles (experiments one through three) is 13% in the wavelength range of 2.5 μm to 25 μm.

[0036] Figure 2 The visible-near-infrared surface reflectance curves of tantalum particles prepared in Experiments 1 to 5 are shown. The dimensions marked by the five curves in the figure are the corresponding particle sizes of the tantalum particles. It can be seen that the reflectance of the three nano-sized tantalum particles (Experiments 1 to 3) is relatively low, all below 10%. Among them, the tantalum nanoparticles prepared in Experiment 2 have an average reflectance of 9.49% in the wavelength range of 250 nm to 2500 nm.

Claims

1. A method for preparing highly absorbent tantalum nanoparticles, characterized in that... The preparation method of high-absorption tantalum nanoparticles is carried out according to the following steps:

1. Cleaning the substrate: First, clean the substrate with high-pressure air for 5 min to 10 min, then use anhydrous ethanol for ultrasonic cleaning for 4 min to 6 min, then use ultrapure water for ultrasonic cleaning for 4 min to 6 min, blow dry with nitrogen, and modify the surface with octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate. II. Pre-sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. −3 Below Pa, fix the tantalum target material, use high-purity argon as the working gas, adjust the temperature of the substrate after step one to 0~200℃, control the sputtering working vacuum at 0.8Pa~1.2Pa, the pre-sputtering power is 10W~50W, and the time is 50s~70s. III. Secondary sputtering: The chamber background vacuum is controlled at 3×10⁻⁶. −3 Below Pa, the working gas is high-purity argon. The substrate temperature is adjusted to 0~200℃, the sputtering working vacuum is controlled at 0.8Pa~1.2Pa, the sputtering power is 50W, and the sputtering time is 2min, so that tantalum nanoparticles are obtained on the substrate. The tantalum nanoparticles have an average reflectance of 9.49% in the wavelength range of 250nm to 2500nm and an average reflectance of 13% in the wavelength range of 2.5μm to 25μm.

2. The method for preparing high-absorption tantalum nanoparticles according to claim 1, characterized in that... The substrate mentioned in step one is a silicon wafer, quartz, or ITO.

3. The method for preparing high-absorption tantalum nanoparticles according to claim 2, characterized in that... In step one, the substrate is first cleaned with high-pressure air for 5 minutes, then ultrasonically cleaned with anhydrous ethanol for 4 minutes, and then ultrasonically cleaned with ultrapure water for 4 minutes.

4. The method for preparing high-absorption tantalum nanoparticles according to claim 1, characterized in that... The method for surface modification with octadecyltrichlorosilane in step one is to sonicate the substrate in a solution of octadecyltrichlorosilane.

5. The method for preparing high-absorption tantalum nanoparticles according to claim 1, characterized in that... In step two, the temperature of the substrate after the treatment in step one is adjusted to 25°C.

6. The method for preparing high-absorption tantalum nanoparticles according to claim 1, characterized in that... In step two, the pre-sputtering power is 15W and the time is 50s.

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