阅读说明：本技术 一种六硼化镱纳米棒晶体的制备方法 (Preparation method of ytterbium hexaboride nanorod crystal ) 是由 童东革 李传奇 周瑞 于 2019-10-23 设计创作，主要内容包括：本发明公开了一种六硼化镱纳米棒晶体的制备方法。本发明通过液相等离子体技术和溶剂热法相结合的方法成功地在130摄氏度的温度下制备出了六硼化镱纳米棒晶体。与商用六硼化镱相比,本发明所制备的六硼化镱纳米棒晶体比表面积更大,抑菌效果更强。与丁胺卡那霉素和卡那霉素相比,本发明所制备的六硼化镱纳米棒晶体对白色念珠菌表现出了更强的抗菌活性。其优异的白色念珠菌抑菌性能有望拓展六硼化镱纳米化合物在医疗器械涂料和直接治疗伤口或烧伤等方面的应用。(The invention discloses a preparation method of ytterbium hexaboride nanorod crystals. The invention successfully prepares the ytterbium hexaboride nanorod crystal at the temperature of 130 ℃ by combining a liquid phase plasma technology and a solvothermal method. Compared with commercial ytterbium hexaboride, the ytterbium hexaboride nanorod crystal prepared by the method is larger in specific surface area and stronger in antibacterial effect. Compared with amikacin and kanamycin, the ytterbium hexaboride nanorod crystal prepared by the invention has stronger antibacterial activity on candida albicans. The excellent candida albicans antibacterial performance of the ytterbium hexaboride nano compound is expected to expand the application of the ytterbium hexaboride nano compound in medical appliance coatings and the aspect of directly treating wounds or burns and the like.)

1. A preparation method of ytterbium hexaboride nanorod crystals is characterized by comprising the following steps: the preparation method comprises the following specific steps:

(1) mixing 3 mmol of ytterbium trichloride, a proper amount of polyethylene glycol and potassium phosphate in 30 ml of ionic liquid, and stirring for 25 minutes under the protection of argon gas to form a solution, wherein the molar ratio of the ytterbium trichloride to the polyethylene glycol is 8-16:1: 0.2-0.7;

(2) transferring the mixed solution obtained in the step (1) into a 60 ml reaction kettle under the protection of argon, introducing diborane to ensure that the molar ratio of the diborane to the ytterbium trichloride is 8-14, and sealing the reaction kettle;

(3) starting liquid phase plasma with the power of 400 plus 800 watts, and treating the mixed solution in the reaction kettle in the step (2) at the temperature of 110 plus 150 ℃ for 60-90 minutes to obtain a crude product of ytterbium hexaboride nanorod crystals;

(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.

2. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (1), the molecular weight of the polyethylene glycol is 6000.

3. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (1), the molar ratio of ytterbium trichloride, polyethylene glycol and potassium phosphate is 12:1: 0.4.

4. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (2), the molar ratio of the introduced diborane to the ytterbium trichloride is 11: 1.

5. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (3), the power of the liquid phase plasma is 600 watts.

6. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (3), the reaction temperature is 130 ℃.

7. The method of preparing ytterbium hexaboride nanorod crystals of claim 1, wherein: in the step (3), the reaction time was 75 minutes.

Technical Field

The invention relates to the technical field of nano materials, in particular to a preparation method of ytterbium hexaboride alloy nanocrystals.

Background

Ytterbium hexaboride crystals are favored in many electronic device engineering applications due to their excellent surface conductivity properties. However, the current synthesis methods of ytterbium hexaboride crystals, such as: the mechanochemical method, the high-temperature sintering method, the vacuum calcination method, the combustion synthesis method and the like are time-consuming and energy-consuming, and the commercialization process is severely limited.

Therefore, it is very necessary to develop a new and efficient method for synthesizing ytterbium hexaboride crystals. At present, the combination of liquid phase plasma technology and solvothermal synthesis method becomes a new synthesis method for synthesizing metal boride nano-crystals. For example, the europium hexaboride nano cubic crystal is successfully synthesized by combining a liquid plasma technology and a solvothermal synthesis method, and the europium hexaboride nano cubic crystal has stronger antibacterial performance of staphylococcus aureus.

Disclosure of Invention

According to the invention, by a strategy of combining a liquid phase plasma technology and a solvothermal synthesis method, polyethylene glycol is used as a surfactant and potassium phosphate is used as a crystal face inducer, and ytterbium hexaboride nanorod crystals are synthesized by reducing ytterbium chloride with diborane at the temperature of 130 ℃ for the first time, wherein the average grain width and the grain length are about 20nm and 80nm respectively, and the ytterbium hexaboride nanorod crystals have excellent anti-candida albicans activity.

The invention adopts the following technical scheme:

(1) mixing 3 mmol of ytterbium trichloride, a proper amount of polyethylene glycol and potassium phosphate in 30 ml of ionic liquid, and stirring for 25 minutes under the protection of argon gas to form a solution, wherein the molar ratio of the ytterbium trichloride to the polyethylene glycol is 8-16:1: 0.2-0.7;

(2) transferring the mixed solution obtained in the step (1) into a 60 ml reaction kettle under the protection of argon, introducing diborane to ensure that the molar ratio of the diborane to the ytterbium trichloride is 8-14, and sealing the reaction kettle;

(3) starting liquid phase plasma with the power of 400 plus 800 watts, and treating the mixed solution in the reaction kettle in the step (2) at the temperature of 110 plus 150 ℃ for 60-90 minutes to obtain a crude product of ytterbium hexaboride nanorod crystals;

(4) washing the product with deionized water for three times, then washing the product with absolute ethyl alcohol for three times, and drying the product for later use.

In the step (1), the molecular weight of the polyethylene glycol is 6000.

In the step (1), ytterbium trichloride is preferable, and the molar ratio of polyethylene glycol to potassium phosphate is 12:1: 0.4.

In the step (2), diborane is preferably introduced into the mixed liquid in the step (1) under the protection of argon and at the molar ratio of the diborane to the ytterbium trichloride of 11:1, and the reaction kettle is sealed.

In the step (3), the power of the liquid phase plasma is preferably 600 watts.

In the step (3), the reaction temperature is preferably 130 ℃.

In the step (3), the reaction time is preferably 75 minutes.

The invention has the following positive effects:

1) the invention successfully synthesizes ytterbium hexaboride nano-rod crystals at the temperature of 130 ℃ for the first time by adopting a method of combining a liquid phase plasma technology and a solvothermal method.

2) Compared with commercial ytterbium hexaboride, the ytterbium hexaboride nanorod crystal synthesized by the method is larger in specific surface area.

3) Compared with commercial ytterbium hexaboride, the ytterbium hexaboride nanorod crystal synthesized by the method has stronger antibacterial activity.

4) Compared with amikacin and kanamycin, the ytterbium hexaboride nanorod crystal synthesized by the method has stronger antibacterial activity on candida albicans.

Drawings

FIG. 1 is a TEM photograph of ytterbium hexaboride nanorod crystals prepared in example 1.

FIG. 2 is a high-power TEM photograph of ytterbium hexaboride nanorod crystals prepared in example 1.

FIG. 3 is a selected-region electron diffraction photograph of ytterbium hexaboride nanorod crystals prepared in example 1.

FIG. 4 is an X-ray diffraction pattern of ytterbium hexaboride nanorod crystals prepared in example 1.

FIG. 5 is Yb4d and B1sXPS spectra of ytterbium hexaboride nanorod crystals prepared in example 1.

FIG. 6 is a Yb4pXPS spectrum of ytterbium hexaboride nanorod crystals prepared in example 1.

Detailed Description

The following examples are further detailed descriptions of the present invention.

The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.

Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.