Preparation method of high-absorption tantalum nanoparticles

Abstract

The invention discloses a preparation method of high-absorption tantalum nanoparticles, belongs to the field of preparation of nanoparticles on the surface of a substrate, and particularly relates to the preparation method of the high-absorption tantalum nanoparticles. The invention aims to solve the technical problems of high cost and large particle size of tantalum nanoparticles prepared at present. The method comprises the following steps: selecting a proper tantalum target material and a substrate, cleaning the substrate, and fixing the substrate in a sputtering chamber; meanwhile, the vacuum degree in the sputtering chamber is adjusted; filling a proper amount of working gas into the sputtering chamber, and applying a high-voltage electric field to ionize the gas; the size, morphology and distribution of the tantalum nanoparticles are controlled by adjusting parameters such as magnetron sputtering power, sputtering time, gas pressure and the like. The tantalum nanoparticles prepared by the method can effectively reduce the reflectivity, the average reflectivity of the tantalum nanoparticles can reach 9.49% within the wavelength of 250-2500nm, and the average reflectivity of the tantalum nanoparticles can reach 13% within the wavelength of 2.5-25mu m.

Description

Technical Field

[0001] The invention belongs to the field of substrate surface nanoparticle preparation, in particular to a method for preparing high-absorption tantalum nanoparticles. Background Art

[0002] Tantalum nanoparticles have unique optical properties, such as wide-area spectral absorption and high photothermal conversion efficiency, which make them potentially useful in photoacoustic imaging, photothermal therapy, and other fields. Tantalum nanoparticles can be used to prepare high-performance composite materials and coating materials to improve the strength, hardness, wear resistance, and other properties of the materials.

[0003] Existing methods for preparing tantalum nanoparticles include chemical vapor deposition (CVD), vacuum plasma spraying (VPS), plasma immersion ion implantation, etc. However, the above preparation methods have the following problems: it is difficult to obtain nanoparticles from the prepared dense tantalum coating film, and the equipment requirements are high and the maintenance cost is high. For example, in the CVD process, some impurities may be introduced due to the contact between the gas and the reactants and the possible cross-contamination of the gas, resulting in a certain degree of non-uniformity. The uniformity and thickness distribution of the particles are difficult to control accurately, and it is difficult to prepare nanoparticles effectively. In addition, plasma immersion ion implantation usually takes a long time to complete an injection process, and requires a large amount of energy to maintain the formation and maintenance of the plasma. In summary, the cost of preparing Ta nanoparticles in the prior art is relatively high, and the particle size of Ta nanoparticles 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 is bombarded by high-energy particles (such as argon ions), so that the atoms or atomic groups on the surface of the target obtain enough energy to break away from the surface of the target, forming sputtered particles. These particles are confined in the plasma region near the target under the action of the magnetic field, and after multiple collisions and scattering, they eventually form nanoparticles on a low surface energy. Summary of the invention

[0005] The present invention aims to solve the technical problems that the cost of preparing tantalum nanoparticles is relatively high and the particle size is relatively large, and to provide a method for preparing high-absorption tantalum nanoparticles.

[0006] The preparation method of 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 minutes to 10 minutes, then use anhydrous ethanol for ultrasonic cleaning for 4 minutes to 6 minutes, then use ultrapure water for ultrasonic cleaning for 4 minutes to 6 minutes, blow dry with nitrogen, and modify the surface with octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate;

[0008] 2. Pre-sputtering: The chamber background vacuum is controlled at 3×10 -3 Pa or less, fix the tantalum target, use high-purity argon as the working gas, adjust the temperature of the substrate after the treatment in step 1 to 0-200°C, control the sputtering vacuum degree at 0.8Pa-1.2Pa, and use the pre-sputtering power at 10W-50W for 50s-70s;

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

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

[0011] 1. The present invention utilizes magnetron sputtering to uniformly prepare tantalum nanoparticles, and the particle size of the tantalum nanoparticles can be regulated by controlling process parameters;

[0012] 2. The tantalum nanoparticles prepared by the present invention can effectively reduce the reflectivity. The average reflectivity can reach 9.49% within the wavelength range of 250nm to 2500nm, and the average reflectivity can reach 13% within the wavelength range of 2.5μm to 25μm.

[0013] 3. The process operation of the present invention can be applied to a variety of substrate materials, such as silicon wafers, quartz and ITO. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 The infrared emissivity curves of the tantalum particles prepared in Experiments 1 to 5 are shown;

[0015] Figure 2 The visible-near infrared spectral surface reflectance curves of the tantalum particles prepared in Experiments 1 to 5. DETAILED DESCRIPTION

[0016] Specific implementation method 1: This implementation method is a method for preparing high-absorption tantalum nanoparticles, which is specifically carried out according to the following steps:

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

[0018] 2. Pre-sputtering: The chamber background vacuum is controlled at 3×10 -3Pa or less, fix the tantalum target, use high-purity argon as the working gas, adjust the temperature of the substrate after the treatment in step 1 to 0-200°C, control the sputtering vacuum degree at 0.8Pa-1.2Pa, and use the pre-sputtering power at 10W-50W for 50s-70s;

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

[0020] Specific implementation method 2: This implementation method is different from specific implementation method 1 in that the substrate described in step 1 is a silicon wafer, quartz or ITO. The rest is the same as specific implementation method 1.

[0021] Specific implementation method 3: This implementation method is different 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 then ultrasonically cleaned with ultrapure water for 4 minutes. The rest is the same as specific implementation method 1 or 2.

[0022] Specific embodiment 4: This embodiment differs from specific embodiments 1 to 3 in that the method for surface modification with octadecyltrichlorosilane in step 1 is to ultrasonically treat the substrate in a solution of octadecyltrichlorosilane. The rest is the same as specific embodiments 1 to 3.

[0023] Specific implementation mode 5: This implementation mode is different from specific implementation mode 4 in that: in step 2, the temperature of the substrate after being processed in step 1 is adjusted to 25° C. The rest is the same as specific implementation mode 4.

[0024] Specific implementation example 6: This implementation example is different from specific implementation example 5 in that the power of the pre-sputtering in step 2 is 15 W and the time is 50 s. The rest is the same as specific implementation example 5.

[0025] Specific embodiment 7: This embodiment differs from specific embodiment 6 in that the sputtering power in step 3 is 50 W and the sputtering time is 2 min. The rest is the same as specific embodiment 6.

[0026] The present invention is verified by the following tests:

[0027] Experiment 1: This experiment is a method for preparing highly absorbent tantalum nanoparticles, which is specifically carried out in the following steps:

[0028] 1. Cleaning the substrate: First, clean the substrate silicon wafer 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 ultrasonically clean the substrate in an octadecyltrichlorosilane solution to obtain a superhydrophobic surface on the substrate;

[0029] 2. Pre-sputtering: The chamber background vacuum is controlled at 3×10 -3 Pa, fix the pure tantalum target, use high-purity argon as the working gas, adjust the substrate temperature after step 1 to 25°C, control the sputtering vacuum degree at 0.8Pa, and pre-sputter power at 15W for 50s;

[0030] 3. Secondary sputtering: The chamber background vacuum is controlled at 3×10 -3 Pa, the working gas is high-purity argon, the substrate temperature is adjusted to 25°C, the sputtering working vacuum is controlled at 0.8Pa, the sputtering power is 50W, the sputtering time is 2min, and the particle size of tantalum nanoparticles prepared on the substrate is 50nm.

[0031] Experiment 2: The difference between this experiment and experiment 1 is that the background vacuum of the chamber in step 2 is controlled at 5×10 -4 Pa, the sputtering vacuum is controlled at 1Pa, and the pre-sputtering power is 25W; in step 3, the chamber background vacuum is controlled at 5×10 -4 Pa, the sputtering vacuum is controlled at 1Pa, the pre-sputtering power is 75W, the sputtering time is 5min, and the particle size of the tantalum nanoparticles prepared on the substrate is 80nm-100nm. Others are the same as experiment 1.

[0032] Experiment 3: The difference between this experiment and experiment 1 is that the background vacuum of the chamber in step 2 is controlled at 5×10 -4 Pa, the substrate temperature after step 1 was adjusted to 50 °C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 25 W, and the time was 70 s; in step 3, the chamber background vacuum was controlled at 5 × 10 -4 Pa, the substrate temperature was adjusted to 50°C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, the sputtering time was 10 min, and the particle size of the tantalum nanoparticles obtained on the substrate was 200 nm to 300 nm. Others were the same as in Experiment 1.

[0033] Experiment 4: The difference between this experiment and experiment 1 is that the background vacuum of the chamber in step 2 is controlled at 5×10 -4 Pa, the substrate temperature after step 1 was adjusted to 100 °C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 25 W, and the time was 20 s; in step 3, the chamber background vacuum was controlled at 5 × 10 -4Pa, the substrate temperature was adjusted to 100°C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, the sputtering time was 15 min, and the particle size of the tantalum particles obtained on the substrate was 10 μm. Others were the same as in Experiment 1.

[0034] Experiment 5: The difference between this experiment and experiment 1 is that the background vacuum of the chamber in step 2 is controlled at 5×10 -4 Pa, the substrate temperature after step 1 was adjusted to 150 ° C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 25 W, and the time was 20 s; in step 3, the chamber background vacuum was controlled at 5 × 10 -4 Pa, the substrate temperature was adjusted to 150°C, the sputtering vacuum was controlled at 1 Pa, the pre-sputtering power was 75 W, the sputtering time was 25 min, and the particle size of the tantalum particles obtained on the substrate was 53 μm. Others were the same as in Experiment 1.

[0035] Figure 1 This is a graph of the infrared emissivity of the tantalum particles prepared in Experiments 1 to 5. The sizes marked by the 5 curves in the figure are the particle sizes of the corresponding tantalum particles. It can be seen that the average reflectivity of the three nanometer-sized tantalum particles (Experiments 1 to 3) in the wavelength range of 2.5μm to 25μm is 13%.

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

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 minutes to 10 minutes, then use anhydrous ethanol for ultrasonic cleaning for 4 minutes to 6 minutes, then use ultrapure water for ultrasonic cleaning for 4 minutes to 6 minutes, blow dry with nitrogen, and modify the surface with octadecyltrichlorosilane to obtain a superhydrophobic surface on the substrate; 2. Pre-sputtering: The chamber background vacuum is controlled at 3×10 -3 Pa or less, fix the tantalum target, use high-purity argon as the working gas, adjust the temperature of the substrate after the treatment in step 1 to 0-200°C, control the sputtering vacuum degree at 0.8Pa-1.2Pa, and use the pre-sputtering power at 10W-50W for 50s-70s; 3. Secondary sputtering: The chamber background vacuum is controlled at 3×10 -3 Pa, the working gas is high-purity argon, the substrate temperature is adjusted to 0-200°C, the sputtering working vacuum is controlled at 0.8Pa-1.2Pa, the sputtering power is 50W-100W, the sputtering time is 2min-10min, and tantalum nanoparticles are obtained on the substrate.

2. The method for preparing highly absorbent tantalum nanoparticles according to claim 1, characterized in that The substrate described in step 1 is silicon wafer, quartz or ITO.

3. The method for preparing highly absorbent tantalum nanoparticles according to claim 2, characterized 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 then ultrasonically cleaned with ultrapure water for 4 minutes.

4. The method for preparing highly absorbent tantalum nanoparticles according to claim 1, characterized in that The method for surface modification with octadecyltrichlorosilane in step 1 is to ultrasonically treat the substrate in a solution of octadecyltrichlorosilane.

5. The method for preparing highly absorbent tantalum nanoparticles according to claim 1, characterized in that In step 2, the temperature of the substrate treated in step 1 is adjusted to 25°C.

6. The method for preparing highly absorbent tantalum nanoparticles according to claim 1, characterized in that In step 2, the pre-sputtering power is 15 W and the time is 50 s.

7. The method for preparing highly absorbent tantalum nanoparticles according to claim 1, characterized in that In step 3, the sputtering power is 50 W and the sputtering time is 2 min.

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