Preparation method of Mg nanoparticles
By adding 1,4-dioxane to adjust the solution properties, controlling the reaction rate, and performing vacuum drying during the preparation of Mg nanoparticles, the problem of large Mg nanoparticle size was solved, and particles of 200-300 nm were prepared, which are suitable for plasmonic sensing and hydrogen storage.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- GUILIN UNIV OF ELECTRONIC TECH
- Filing Date
- 2026-03-23
- Publication Date
- 2026-05-15
AI Technical Summary
The Mg nanoparticles prepared by existing technologies are relatively large in size, which makes it difficult to meet the application requirements of certain fields.
Mg nanoparticles were prepared by adjusting the solution viscosity and polarity and controlling the reaction rate by adding 1,4-dioxane during the reaction process, combined with a vacuum drying step.
The size of Mg nanoparticles was successfully reduced to about 200-300 nm, meeting the application requirements of plasmon sensing, medicine and hydrogen storage.
Smart Images
Figure CN122033263A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the technical field of hydrogen storage materials, and specifically to a method for preparing Mg nanoparticles. Background Technology
[0002] Magnesium and its alloys, due to their low density and high specific strength, show great potential for applications in aerospace, automotive lightweighting, and other fields. When magnesium reaches the nanoscale, its surface and quantum effects exhibit unique properties distinct from bulk materials, leading to its use in plasmonic sensing, medicine, and hydrogen storage. Currently, magnesium nanoparticles prepared by solution methods are often quite large. This invention aims to reduce the size of the prepared magnesium nanoparticles by adding an organic solvent during the reaction process. Summary of the Invention
[0003] In view of the shortcomings of the prior art described above, the present invention provides a method for preparing Mg nanoparticles and controlling their size, which solves the problem of large size of Mg nanoparticles prepared in the prior art.
[0004] To achieve the above and other related objectives, the method for preparing Mg nanoparticles of the present invention is implemented through the following technical solution:
[0005] Step S1: Add lithium particles and naphthalene to tetrahydrofuran and stir to obtain solution A;
[0006] Step S2: Add n-dibutylmagnesium to solution A, then add 1,4-dioxane, and stir for a period of time to obtain solution B;
[0007] Step S3: Using tetrahydrofuran as the washing solution, the reaction product is centrifuged and washed under certain conditions;
[0008] Step S4: Vacuum drying under certain conditions yields Mg nanoparticles.
[0009] Furthermore, in the preparation method of the Mg nanoparticles, the molar ratio of lithium, naphthalene, and n-dibutylmagnesium is 2:2:1, and the volume ratio of tetrahydrofuran and 1,4-dioxane is 1:1.
[0010] Furthermore, in the preparation method of the Mg nanoparticles, the solution reaction conditions are: reaction temperature of 20-25℃ and reaction time of 3h; the centrifugation washing conditions are: centrifugation speed of 7000 rpm, centrifugation time of 20 min, and centrifugation times of 3; the drying conditions are: drying temperature of 50-70℃ and drying time of 8-12h.
[0011] Furthermore, in the method for preparing Mg nanoparticles, the entire reaction is carried out in a glove box filled with argon gas.
[0012] The beneficial effects of this invention are:
[0013] The size of the prepared Mg nanoparticles was reduced by adjusting the solution viscosity and polarity through the addition of 1,4-dioxane and by reducing the reaction rate through reaction with the reactants. Attached Figure Description
[0014] The accompanying drawings, which are included to provide a further understanding of the embodiments of the present invention and form part of this application, do not constitute a limitation on the embodiments of the present invention.
[0015] Figure 1 The image shows the XRD pattern of the Mg nanoparticles prepared in this invention.
[0016] Figure 2 This is a TEM image of the Mg nanoparticles prepared in this invention. Detailed Implementation
[0017] The present invention will be further described in detail through embodiments and with reference to the accompanying drawings, but this is not intended to limit the scope of the invention.
[0018] Example 1
[0019] 0.0281 g of lithium particles and 1.0587 g of naphthalene were added to 20 ml of tetrahydrofuran and stirred for 1 h to obtain solution A. Then, 4 ml of n-dibutylmagnesium was added to solution A, followed by 20 ml of 1,4-dioxane, and the mixture was stirred for 3 h to obtain solution B. Solution B was centrifuged and washed three times with tetrahydrofuran as the washing solution to remove byproducts. Finally, the solution was vacuum dried at 60 °C to obtain Mg nanoparticles.
[0020] Comparative Example 1
[0021] 0.0281 g of lithium particles and 1.0587 g of naphthalene were added to 40 ml of tetrahydrofuran and stirred for 1 h to obtain solution A. Then, 4 ml of n-dibutylmagnesium was added to solution A and stirred for 3 h to obtain solution B. Solution B was centrifuged and washed three times with tetrahydrofuran as the washing solution to remove byproducts. Finally, it was vacuum dried at 60 °C to obtain Mg nanoparticles.
[0022] To obtain the phase composition of the prepared nanoparticles, XRD analysis was performed. The test results are as follows: Figure 1 As shown, Sample 1 was prepared without the addition of 1,4-dioxane, and Sample 2 was prepared with the addition of 1,4-dioxane. The diffraction peaks of the nanoparticles prepared in Example 1 and Comparative Example 1 are consistent with the characteristic diffraction peaks of Mg, and no other phase diffraction peaks are present. The test results indicate that the nanoparticles prepared in Example 1 and Comparative Example 1 are all elemental Mg.
[0023] TEM measurements were performed to obtain the size and morphology of the Mg nanoparticles. The test results are as follows: Figure 2 As shown, (a) is the sample prepared without the addition of 1,4-dioxane, and (b) is the sample prepared with the addition of 1,4-dioxane. The sample prepared without the addition of 1,4-dioxane has a size of about 1 µm, while the sample prepared with the addition of 1,4-dioxane has a size of 200-300 nm.
Claims
1. A method for preparing Mg nanoparticles, characterized in that, Includes the following steps: Step S1: Add lithium particles and naphthalene to tetrahydrofuran and stir for 1 hour to obtain solution A; Step S2: Add n-dibutylmagnesium to solution A, then add 1,4-dioxane, and stir for a period of time to obtain solution B; Step S3: Using tetrahydrofuran as the washing solution, the reaction product is centrifuged and washed under certain conditions; Step S4: Vacuum drying under certain conditions yields Mg nanoparticles.
2. The method for preparing Mg nanoparticles according to claim 1, characterized in that: The molar ratio of lithium, naphthalene, and dibutylmagnesium is 2:2:1, and the volume ratio of tetrahydrofuran in step S1 to 1,4-dioxane in step S2 is 1:
1.
3. The method for preparing Mg nanoparticles according to claim 1, characterized in that: The conditions for the solution reaction are as follows: in step S2, the reaction temperature is 20-25℃ and the reaction time is 3h; the conditions for centrifugation and washing are as follows: the centrifugation speed is 7000 rpm, the centrifugation time is 20min, and the number of centrifugations is 3; in step S4, the conditions for drying are as follows: the drying temperature is 50-70℃ and the drying time is 8-12h.
4. The method for preparing Mg nanoparticles according to claim 1, characterized in that: The entire reaction was carried out in a glove box filled with argon gas.