CN101538032B - Method for preparing high-concentration stable carbon nano-tube aqueous solutions - Google Patents

Abstract

The invention discloses a method for preparing high-concentration stable carbon nano-tube aqueous solution. The method comprises the steps of using an ultrasonic probe to oxidize carbon nano-tubes in a mixed strong-acid solution, filtering the solution, washing and drying filtered substances, using the ultrasonic probe to disperse the dried filtered substances in water and obtaining a uniform stable black solution. The method does not need to introduce surfactant, and the concentration of the carbon nano-tubes in the obtained aqueous solution reaches up to 0.5 mg/ml. Observation under a scanning electron microscope shows that most of the carbon nano-tubes in the solution are open in state and clear in tubular structure, and hollow tubular structures are maintained well. Dynamic light scattering test shows that the carbon nano-tubes are about 140 nanometers in mean effective diameter and 70 to 350 nanometers in distribution range. The stability of the carbon nano-tube aqueous solution prepared by the method can reach two weeks. The method provides guarantee for the further application of the carbon nano-tubes in the field of biological medicine.

Description

Method for preparing high-concentration stable carbon nanotube aqueous solution

Technical field:

The invention relates to a preparation method and application of a carbon nanotube aqueous solution used in the field of biomedicine.

Background technique:

Carbon nanotubes are a class of tubular carbon materials with a perfect graphite structure, and their diameters generally range from a few nanometers to tens of nanometers. Carbon nanotubes have excellent electrical conductivity, electromagnetic properties and excellent mechanical properties. It has a variety of excellent properties and has broad application prospects in many aspects. However, carbon nanotubes in the original state have strong hydrophobicity, and there is a strong agglomeration effect between them, so it is difficult to disperse in water, organic solvents, and polymer matrices, and they are easy to aggregate into clusters, generally insoluble in any solvent , which hinders its molecular level research and operational application, and it is also difficult to apply it to the field of biomedicine.

In order to apply the excellent properties of carbon nanotubes to the field of biomedicine, surface treatment of carbon nanotubes to disperse them in water and form a stable suspension of carbon nanotubes is of great significance for further biomedical applications. What method to use to modify and functionalize carbon nanotubes has become a key issue for carbon nanotubes to be practical.

The ports of pristine carbon nanotubes are closed. Under certain conditions, some lattice defects exist on the surface of carbon nanotubes. Many studies have used oxidation methods to change the ports of carbon nanotubes from a closed state to an open state, and at the same time oxidized at lattice defects, and introduced oxygen-containing groups such as carboxyl groups on the ports and surfaces of carbon nanotubes to increase the hydrophilicity of carbon nanotubes. .

So far, the most widely used method for hydrophilic modification of carbon nanotubes is the covalent modification method. The commonly used covalent modification method is to oxidize the opening of carbon nanotubes with strong acid, and cut them into short tubes, so that carboxyl groups are attached to the defect sites on the ends or (and) side walls. For example, carbon nanotubes can be turned into an open state by reflux in hot nitric acid solution for a long time to increase their water solubility; there is also a long-term treatment with a mixed solution of concentrated sulfuric acid and nitric acid, assisted by ultrasound, to make single-walled carbon nanotubes The tubes are cut short to 100-300nm, and carboxyl groups are introduced into the surface, which increases the solubility of carbon nanotubes in aqueous solution (J.Liu, A.G.Rinzler, H.Dai, J.H.Hafher, R.K.Bradley, P.J.Boul, A.Lu, T. Iverson, K. Shelimov, C.B. Huffman, F. Rodriguez-Macias, Y.-S. Shon and T.R. Lee D.T. Colbert, R.E. Smalley Fullerene Pipescience 1998, 280, 1253-56). The Mitra S research group used microwaves and mixed strong acids to disperse SWNTs (Wang, Y, Iqbal, Z., Mitra, S.J. Rapidly Functionalized, Water-Dispersed Carbon Nanotubes at High Concentration J.Am.Chem.Soc.2006, 128(1), 95 -99.), carboxyl and sulfonic acid groups were introduced on the surface of carbon nanotubes to obtain a high-concentration carbon nanotube aqueous solution. After surface element analysis, it was found that every 3 carbon atoms introduced a carboxyl group, and every 10 carbon atoms introduced a sulfonic acid group. Scanning electron microscopy observed that the diameter of carbon nanotubes became slightly smaller. Laser dynamic light scattering analysis shows that the particle size in the solution is in the range of 3 nm to 800 nm.

In addition to the oxidation method, some other methods have also been used to disperse carbon nanotubes into aqueous solutions. For example, by wrapping water-soluble macromolecules around carbon nanotubes, full-length carbon nanotubes can be dispersed into solution (Zorbas V, Smith AL, Xie H, Ortiz-Acevedo A, Dalton AB, DieckmannGR, Draper RK, Baughman RH, Musselman IH Importance of Aromatic Content for Peptide/Single-Walled Carbon Nanotube Interactions J Am Chem Soc.2005 Sep5; 127( : 12323-8). There are also research groups reporting that a stable single-walled carbon nanotube solution can be obtained by using albumin as a dispersant under ultrasonic conditions (Karajanagi SS, Yang H, Asuri P, Sellitto E, Dordick JS, Kane RS Protein-assisted solubilization of single -walled carbon nanotubes Langmuir. 2006 Feb 14;22(4):1392-5). There are also research groups using DNA molecules to modify and disperse carbon nanotubes.

So far, most concentrated acid ultrasonic modification methods (Nanotubes from Surface Modification JAm Chem Soc. 2002 Oct 23; 124(42): 12418-9; Lee GW, Kumar S Dispersion of NitricAcid-Treated SWNTs in Organic Solvents and Solvent Mixtures .Effect ofnicotinamide and urea on the solubility of riboflavin in various solvents. J Phys ChemB Condens Matter Mater Surf Interfaces Biophys. 2005 Sep 15; 109(36): 17128-33; LuQ, Keskar G, Ciocan Rath, Rao R R, ., Rao AM., Larcom LL.Determination of Carbon Nanotube Density by Gradient Sedimentation J Phys Chem B.2006 Dec7; 110(48): 24371-6) The concentration of the carbon nanotube aqueous solution obtained is still relatively low, generally at 0.01～0.2mg /ml, and usually requires the assistance of surfactants or biomacromolecules.

Invention content:

The purpose of the present invention is to make up for the gaps in the prior art, and to provide a method for preparing a high-concentration and stable carbon nanotube aqueous solution and the high-concentration and stable carbon nanotube prepared by the method without introducing a surfactant aqueous solution.

The invention provides a method for preparing a high-concentration and stable carbon nanotube aqueous solution, which is to oxidize the carbon nanotubes in a mixed strong acid solution with an ultrasonic probe, filter and wash the filtrate, and dry the filtrate, then place it in the A uniform and stable black solution was obtained after dispersion treatment with an ultrasonic probe in water.

Wherein, the ratio of the diameter of the ultrasonic probe to the volume of the mixed solution is 1:20-100.

The mixed strong acid solution is prepared from concentrated sulfuric acid and concentrated nitric acid in a ratio of 2:1; the ratio of the weight of the carbon nanotube to the volume of the mixed acid ranges from 1:5 to 2:1 (mg:ml).

The drying refers to drying the filtrate to a constant weight, and the drying temperature ranges from room temperature to 70°C.

The washing of the filtrate refers to washing the filtrate with water until the filtrate is neutral.

The working time of the ultrasonic probe for the oxidation treatment is 30s-12000s, and the working power is 500w-1200w; the working time of the ultrasonic probe for the second dispersion treatment is 10s-15000s, and the working power is 200w-1200w.

Specifically, the method includes the following steps:

1) adding carbon nanotubes to the mixed acid solution, and performing oxidation treatment with an ultrasonic probe to obtain a dark black solution;

2) filter the black solution, wash the filtrate until the filtrate is neutral;

3) drying the filtrate to a constant weight into powder;

4) Add the powder into water, and disperse with an ultrasonic probe to obtain a black solution that is an aqueous solution of carbon nanotubes.

Wherein, the ratio of the carbon nanotubes to the mixed acid solution is 1:0.8-1.5, the volume ratio of the diameter of the ultrasonic probe to the mixed solution is 1:20-30, and the drying temperature is 60-70°C. The working time for the oxidation treatment of the ultrasonic probe is 30s-60s, and the working power is 1000w; the working time for the second dispersion treatment of the ultrasonic probe is 10s-60s, and the working power is 1000w.

The present invention provides a high-concentration stable carbon nanotube aqueous solution, which is prepared by the above method. The carbon nanotube aqueous solution satisfies the following conditions: the concentration is greater than 0.2mg/ml and less than or equal to 0.5mg/ml, and The solution is stable for at least 2 weeks.

The present invention adopts the method of combining concentrated acid oxidation and ultrasound to process carbon nanotubes, and can prepare high-concentration and stable carbon nanotube aqueous solution under the condition of not introducing surfactants. Experimental verification, using the method of the present invention , an aqueous solution with a concentration of carbon nanotubes as high as 0.5 mg/ml can be obtained; observation under a scanning electron microscope shows that the carbon nanotubes are mostly in an open state, and the length of the carbon nanotubes changes from the original 50 μm to 200-1000 nm. About 30nm, the tubular structure is clear, and the hollow tubular structure is well maintained; dynamic laser light scattering test shows that the average effective diameter of carbon nanotubes is about 140nm, and the distribution range is 70-350nm; No obvious carbon nanotube aggregates were observed, the absorbance value of the suspension at 253nm ultraviolet did not change, and the stability could reach 2 weeks.

Description of drawings:

Figure 1 is a photo of the dispersion state of carbon nanotubes in water; in the left picture, A is the state of dispersion of multi-walled carbon nanotubes in water treated with an ultrasonic tank; B is the aqueous solution of multi-walled carbon nanotubes obtained after ultrasonic treatment with a probe . The picture on the right shows carbon nanotube aqueous solutions with different concentrations prepared by mixed strong acid oxidation combined with ultrasonic treatment; among them, the carbon nanotube aqueous solution with a concentration of 0.5mg/ml is in the No. tube aqueous solution, the No. 3 cup is a carbon nanotube aqueous solution with a concentration of 0.05mg/ml.

Fig. 2 is the absorption spectrum of the multi-walled carbon nanotube aqueous solution of the present invention.

Figure 3 is an electron micrograph of multi-walled carbon nanotubes deposited from an aqueous solution. Among them (a) electron micrograph of insufficiently oxidized multi-walled carbon nanotubes; (b) electron micrograph of appropriately oxidized multi-walled carbon nanotubes; (c) electron micrograph of over-oxidized multi-walled carbon nanotubes.

Fig. 4 is the size distribution of multi-walled carbon nanotubes in the carbon nanotube aqueous solution of the present invention (measured by dynamic light scattering method).

Detailed ways:

The preparation of the high-concentration stable carbon nanotube aqueous solution of the present invention adopts the method that the combination of mixed concentrated acid oxidation and ultrasound is used to process the carbon nanotubes. ml) stable carbon nanotube aqueous solution. Specific steps are as follows:

1. Surface oxidation treatment of carbon nanotubes:

Prepare a mixed strong acid solution of concentrated sulfuric acid and concentrated nitric acid. Weigh an appropriate amount of multi-walled carbon nanotubes and add them to the mixed acid solution. After a certain time of treatment with an ultrasonic probe of appropriate diameter, a deep black solution was obtained. After diluting with water, filter (the pore size of the filter membrane is 2 μm), and repeatedly rinse the filtrate until the filtrate is neutral. Dry the filtered carbon nanotube powder to constant weight.

2. Preparation of carbon nanotube aqueous solution:

A certain amount of the above-mentioned carbon nanotubes was weighed and added into pure water, and treated with an ultrasonic probe of an appropriate diameter for a certain period of time to obtain a uniform and stable black solution.

The method will be described in detail below in conjunction with specific examples.

Embodiment 1. Preparation of a carbon nanotube solution with a concentration of 0.5 mg/ml

1) Preparation of mixed acid: prepare concentrated sulfuric acid and concentrated nitric acid in a ratio of 2:1 to form a mixed strong acid solution;

2) Weigh 200 mg of multi-walled carbon nanotubes and add them to 400 ml of mixed acid solution, insert an ultrasonic probe with a diameter of 15 mm into the multi-walled carbon nanotubes and mixed acid, and perform ultrasonic treatment at 1000 w for 2 minutes to obtain a dark black solution.

3) Dilute the dark black solution with water and filter it (the pore size of the filter membrane is 2 μm), rinse the filtrate repeatedly with water until the filtrate is neutral; dry the filtered precipitate at 60°C for about 48 hours to a constant weight to obtain a powder.

4) Weigh 5 mg of the above powder into 10 ml of pure water, and use an ultrasonic probe with a diameter of 6 mm for another 2 minutes to obtain a uniform and stable black solution, which is an aqueous solution of carbon nanotubes with a concentration of 0.5 mg/ml.

Embodiment 2, the preparation concentration is the carbon nanotube solution of 0.4mg/ml

1) The same steps as in Example 1 were adopted, wherein 100 mg of carbon nanotubes were added to 200 ml of mixed acid, the diameter of the probe was 10 mm, and the power of 800 w was ultrasonically treated for 2 minutes to obtain a deep black solution.

2) Dilute the dark black solution with water and filter it (the pore size of the filter membrane is 2 μm), rinse the filtrate repeatedly with water until the filtrate is neutral; dry the filtered precipitate at 70°C for 48 hours to a constant weight to obtain a powder.

3) Weigh 4 mg of the above powder into 10 ml of pure water, and use an ultrasonic probe with a diameter of 6 mm for another 2 minutes to obtain a uniform and stable black solution that is an aqueous solution of carbon nanotubes with a concentration of 0.4 mg/ml.

Embodiment three, the preparation concentration is the carbon nanotube solution of 0.3mg/ml

1) The same steps as in Example 1 were adopted, wherein 200 mg of carbon nanotubes were added to 300 ml of mixed acid, the diameter of the probe was 15 mm, and the power of 1000 w was ultrasonically treated for 2 minutes to obtain a deep black solution.

2) Dilute the dark black solution with water and filter it (the pore size of the filter membrane is 2 μm), rinse the filtrate repeatedly with water until the filtrate is neutral; dry the filtered precipitate at room temperature to a constant weight to obtain a powder.

3) Weigh 3 mg of the above powder into 10 ml of pure water, and use an ultrasonic probe with a diameter of 6 mm for another 2 minutes to obtain a uniform and stable black solution, which is an aqueous solution of carbon nanotubes with a concentration of 0.3 mg/ml.

In the above specific implementation, by adjusting the ratio of step 3) powder and water, carbon nanotube aqueous solutions with different concentrations can be obtained, and carbon nanotube aqueous solutions with lower concentrations such as 0.01mg/ml～0.2mg/ml can also be easily obtained , so no examples are given.

For the aqueous solution of carbon nanotubes obtained in the present invention, the composition of the solution is also determined through spectral scanning analysis, the morphology of the carbon nanotubes in the solution is investigated by a scanning electron microscope, and the size distribution of the carbon nanotubes in the aqueous solution is detected with a dynamic light scattering instrument. The stability of the solution is monitored by the UV absorbance value, so as to check the effectiveness of the method for preparing the carbon nanotube aqueous solution as a whole.

Specifically, the carbon nanotube aqueous solution prepared by the above method is analyzed as follows:

(1) Use ultraviolet/visible/near-infrared spectrophotometer to carry out spectral scanning analysis on the carbon nanotube aqueous solution, the scanning range is set to 190nm to 1400nm, and the interval of scanning wavelength is 0.5nm, before the experiment is carried out, use pure water as the See, Balance Scan Baseline. Add an appropriately diluted carbon nanotube aqueous solution into the sample cell for scanning, and the scanning time is about 30 minutes each time to obtain the spectrum of carbon nanotubes. If there is a characteristic absorption peak at 253nm, it can be confirmed that the prepared product is carbon nanotubes aqueous solution.

Results: The aqueous solution with a concentration of 0.01-0.5mg/ml prepared by the present invention has a characteristic absorption peak at 253nm, which can be confirmed as an aqueous solution of carbon nanotubes. The scanning results of the spectra are shown in Figure 2.

(2) The morphology of the treated carbon nanotubes was observed with a scanning electron microscope. Soak the silicon wafer in acetone for 2 minutes, then soak it in ethanol for 5 minutes, and dry it in an ultra-clean bench. Draw the appropriately diluted carbon nanotube aqueous solution, drop it on the front of the silicon wafer, and dry it in the ultra-clean workbench. The morphology of carbon nanotubes was directly observed with a scanning electron microscope.

Observation results: Refer to the picture (b) in Figure 3, which shows the morphology of carbon nanotubes in the 0.5mg/ml carbon nanotube aqueous solution. It can be seen that the carbon nanotubes basically maintain a single form, and many carbon nanotubes are in an open state. , the length of carbon nanotubes changed from the original 50 μm to 200-1000 nm, the tube diameter was about 30 nm, the tubular structure was clear, and the hollow tubular structure was well maintained.

(3) The dynamic size distribution of carbon nanotubes in aqueous solution was detected by a dynamic light scattering instrument. Put the appropriately diluted carbon nanotube aqueous solution into the laser dynamic light scattering sample cell. After the solution is stable, use a 690nm laser for continuous detection for three minutes. The particle size distribution of the particles obtained within three minutes is passed through a computer program (90Plus Particle Size software, Ver.3.48) to obtain the dynamic particle size distribution curve of the carbon nanotubes in the aqueous solution after analysis.

Experimental results: See Figure 4, which shows that the average effective diameter of carbon nanotubes is about 140nm, and the distribution range is 70-350nm.

(4) Stability experiment

The carbon nanotube solution has a characteristic absorption at 253nm, and the intensity of the absorption peak is linearly related to the concentration of carbon nanotubes in the solution, that is, the larger the OD value, the higher the concentration of carbon nanotubes in the solution. Using this feature, the OD value of the carbon nanotube aqueous solution with a concentration of 0.5 mg/ml was detected at different times. After finding that the room temperature is placed for two weeks, the OD value of the solution does not change, and as the standing time prolongs, such as after being placed at room temperature for one month, the OD value of the solution will decrease, and the method of step 3) in the embodiment is used again for ultrasonic treatment After that, the carbon nanotubes in the solution can be redispersed and the OD value increases. In addition, after the above carbon nanotube solution was left at room temperature for 2 weeks, no obvious carbon nanotube aggregates were observed with the naked eye.

Using the above-described preparation method and inspection method, the present invention has carried out an optimization test on the process of the prepared carbon nanotube aqueous solution, and the results show that: in the preparation process, it is very important to select an ultrasonic probe instead of an ultrasonic tank. In addition, ultrasonic The diameter of the probe and the volume ratio of the mixed acid solution, the weight of carbon nanotubes and the volume ratio of the mixed acid, the dry state of the filtrate, and the ultrasonic assistance when preparing the aqueous solution are also important influencing factors.

Optimization experiment 1: When ultrasonic technology is used to treat carbon nanotubes dispersed in mixed acid, it is difficult to obtain the ideal oxidation effect when the carbon nanotube solution of mixed acid is placed in an ultrasonic bath, and it will be difficult to prepare the aqueous solution. As a result, the concentration of carbon nanotubes in the solution is very low, usually below 0.01 mg/ml.

However, the present invention selects the ultrasonic probe, so that the highest concentration of carbon nanotubes in the aqueous solution can reach 0.5 mg/ml. Referring to Fig. 1, A on the left side of Fig. 1 is the dispersion state of the multi-walled carbon nanotubes ultrasonically treated with an ultrasonic bath; B is the aqueous solution of multi-walled carbon nanotubes obtained after ultrasonic treatment with a probe. The picture on the right shows carbon nanotube aqueous solutions with different concentrations prepared by mixed strong acid oxidation combined with ultrasonic treatment. The solution in the No. 1 cup is the carbon nanotube aqueous solution with a concentration of 0.5 mg/ml, while the No. For the carbon nanotube solution, the No. 3 cup is a carbon nanotube solution with a concentration of 0.05mg/ml. The concentration difference can also be judged from the color of the solution.

Optimization experiment 2: The diameter of the ultrasonic probe and the volume ratio of the mixed acid solution are one of the important factors affecting the oxidation degree, dispersion effect, and maintenance of the tubular structure of carbon nanotubes. When the diameter of the ultrasonic probe is less than 1:100 (mm:ml) relative to the volume of the solution, the diameter of the ultrasonic probe is too small. From the scanning electron microscope to observe the morphology of carbon nanotubes, it is found that most of the carbon nanotubes have not been oxidized and cut. Short, agglomerated distribution (see picture a in Figure 3), indicating that the desired degree of oxidation has not been achieved, and the final carbon nanotubes cannot be dispersed in water, and the concentration of carbon nanotubes in the aqueous solution is usually below 0.01mg/ml; If the diameter of the ultrasonic probe is greater than 1:20 relative to the volume of the solution, the diameter of the ultrasonic probe is too large at this time, and it is found that the tube shape of the carbon nanotubes is destroyed and becomes granular and aggregated (see picture c in Figure 3), indicating oxidation. If the degree is too high, the tubular structure of carbon nanotubes will be destroyed.

Optimization experiment 3: The ratio of the weight of carbon nanotubes to the volume of the mixed acid is one of the factors that affect the oxidation degree of carbon nanotubes. When the volume of mixed acid is too low, the oxidation degree of carbon nanotubes will be low, and the concentration of carbon nanotubes in the final aqueous solution is very low; when the volume of mixed acid is too high, the oxidation degree of carbon nanotubes will be too high, and carbon nanotubes Agglomerated in granular form. The optimization experiment finally determined that the effective ratio range between the weight of carbon nanotubes and the volume of mixed acid was 1:5-2:1 (mg:ml).

Optimization Experiment 4: The carbon nanotubes after oxidation treatment need to be kept dry. The same oxidized carbon nanotubes can be prepared into an aqueous solution after sufficient drying to obtain a high-concentration stable aqueous solution, while carbon nanotubes that have not been fully dried are difficult to disperse into water again. The concentration of carbon nanotubes in the aqueous solution is usually 0.01mg/ below ml. In the present invention, drying to a constant weight is used as a measure of sufficient drying, and the drying temperature is room temperature to 70° C., and the drying time varies with different drying temperatures.

Optimization Experiment 5: When preparing an aqueous solution of carbon nanotubes, for the same oxidized carbon nanotubes, the use of ultrasonic assistance can quickly redisperse the carbon nanotubes into the aqueous solution to form a stable high-concentration aqueous solution; without the use of ultrasonic assistance , carbon nanotubes are difficult to completely disperse in water, and only a very low concentration and unstable aqueous solution can be obtained.

The process and influencing factors for the preparation of high-concentration and stable carbon nanotube aqueous solutions of the present invention have been described in detail above. It can be understood that the examples are only used to illustrate the preparation process and do not constitute limitations to the present invention. The data, pictures and The written descriptions are all obtained based on real experiments, and are also the results of the specific implementation of the present invention, which should constitute the disclosure of the present invention and the support for the technical solution of the present invention.

Claims (5)

1. method for preparing high-concentration stable carbon nano-tube aqueous solutions, be after carbon nanotube is carried out oxide treatment, filtration and washing and leaches thing and oven dry and leach thing with ultrasound probe in mixed strong acids solution with its in water with obtaining uniform and stable dark solution after the ultrasound probe dispersion treatment; The working hour that ultrasound probe carries out oxide treatment is 30s～12000s, and operating power is 500w～1200w, and the working hour that ultrasound probe carries out dispersion treatment is 10s～15000s, and operating power is 200w～1200w; Wherein:

Said mixed strong acids solution is prepared by 2: 1 volume ratio by the vitriol oil and concentrated nitric acid and is formed;

The volume ratio scope of said carbon nanotube weight and mixed strong acids is 1mg: 5ml～2mg: 1ml;

The concentration of said high-concentration stable carbon nano-tube aqueous solutions is between being less than or equal between the 0.5mg/ml more than or equal to 0.3mg/ml, and at least 2 weeks of steady time of solution.

2. according to the said method of claim 1, it is characterized in that said oven dry is meant and is dried to constant weight with leaching thing, said drying temperature scope is room temperature～70 ℃.

3. according to the said method of claim 1, it is characterized in that said washing leaches thing and is meant that water will leach thing washing to filtrating for neutral.

4. according to the said method of claim 1, it is characterized in that, specifically may further comprise the steps:

1) carbon nanotube is added in the mixed strong acids solution, carries out oxide treatment, obtain aterrimus solution with ultrasound probe;

2) aterrimus solution is filtered, washing leaches thing to filtrating for neutral;

3) will leach thing dries to the constant weight powdered;

4) powder is added to the water, carries out dispersion treatment, obtain dark solution and be carbon nano-tube aqueous solutions with ultrasound probe.

5. according to the said method of claim 4, it is characterized in that said carbon nanotube and mixed strong acids solution proportion are 1mg: 0.8～1.5ml, the working hour that said ultrasound probe carries out oxide treatment is 30s～60s, and operating power is 1000w; The working hour that said ultrasound probe carries out dispersion treatment is 10s～60s, and operating power is 1000w.

Images