Preparation method of three-dimensional semiconductor GaN nanoflower material

Abstract

The invention is suitable for the technical field of semiconductor material synthesis, and provides a preparation method of a three-dimensional semiconductor GaN nanoflower material, according to the method, a solvothermal method is utilized to synthesize the three-dimensional tunable GaN nanoflower material which is stable in crystal structure, low in sample cost and environment-friendly, and the tunable GaN nanoflower material is obtained by controlling the reaction time. The obtained three-dimensional GaN nanoflower has a relatively large specific surface area and abundant active sites. In addition, the GaN nanoflower material increases the specific surface area, improves the electron transmission performance, improves the catalytic performance and enhances the light absorption performance, and shows remarkable performance advantages in the fields of photocatalysis, electrocatalysis, gas sensors, optoelectronic devices and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of semiconductor material synthesis, and in particular relates to a method for preparing a three-dimensional semiconductor GaN nanoflower material. Background Art

[0002] Gallium nitride (GaN) is a typical wide bandgap semiconductor material. It has excellent bandgap width (~3.4eV), high thermal conductivity (~130W / m·K), high electron mobility (~1000cm 2 / V·s), chemical stability and radiation resistance, and has a wide range of applications in optoelectronic devices, high-power electronic devices, and catalysis. However, traditional GaN materials mostly exist in the form of thin films or one-dimensional nanostructures (such as nanowires and nanorods), which are difficult to meet the needs of some high-performance devices for high specific surface area, excellent charge transfer performance and enhanced light absorption capacity. In contrast, the three-dimensional nanoflower-like GaN structure, due to its special layered flake or branch-like morphology, exhibits a higher specific surface area, better carrier transfer capacity and stronger light absorption capacity, which is expected to enhance the application value of GaN in optoelectronic devices, photocatalysis, energy storage and other fields.

[0003] Although three-dimensional GaN nanoflower materials have great potential in application, their preparation process is still challenging. The main problems are as follows: (1) Difficulty in synthesis: The high melting point and strong covalent bonds of GaN make its synthesis difficult, especially at low temperatures. Controlling the morphology and size of GaN nanoflowers is even more challenging; (2) Strict morphology control: To accurately control the morphology of GaN nanoflowers (such as the number, size, and distribution of petals), it is necessary to adjust the synthesis conditions, such as temperature, precursor concentration, and reaction time; (3) High cost: The preparation cost of GaN materials is relatively high, especially in large-scale production. Reducing costs remains an urgent problem to be solved. Summary of the invention

[0004] The purpose of the embodiments of the present invention is to provide a method for preparing a three-dimensional semiconductor GaN nanoflower material, aiming to solve the problems raised in the above background technology.

[0005] The embodiment of the present invention is implemented as follows: a method for preparing a three-dimensional semiconductor GaN nanoflower material comprises the following steps:

[0006] Step 1: Pour 2 ml of octadecene into a three-necked flask, connect the system, and degas for 15 min at room temperature;

[0007] Step 2: Raise the reaction temperature to 120°C, degas for 20 min, and then cool down to 60°C in a N2 atmosphere;

[0008] Step 3: Rapidly inject 2 ml of lithium bis(trimethylsilyl)amide and degas at room temperature for at least 20 min;

[0009] Step 4: degassing at 120 °C for 20 min under N2 atmosphere, cooling to 60 °C to obtain a ligand solution;

[0010] Step 5: 88 mg of gallium chloride, 0.478 ml of oleylamine and 5 ml of octadecene were placed in a three-necked flask;

[0011] Step 6: After degassing at 120°C for 15 min, the temperature was raised to 320°C in a N2 atmosphere;

[0012] Step 7: Rapidly inject 1.5 ml of the ligand solution in step 6, and react for 15 seconds to obtain GaN-15s;

[0013] Step 8: The obtained solution was washed with n-hexane, methanol, ethanol and acetone respectively and centrifuged;

[0014] Step 9: Place the powder obtained after washing in a vacuum drying oven for drying to obtain a three-dimensional GaN-15s nanoflower product.

[0015] According to a further technical solution, in step 1, octadecene is 1-Octadecene, which is injected into a three-necked flask using a pipette.

[0016] According to a further technical solution, in step 1 and step 5, a magnet is added into the three-necked flask, and the rotation speed of the magnet in the solution is 660 rpm.

[0017] A further technical solution is that in step 3, a bis(trimethylsilyl)amide lithium solution (5.32 mol / L) is rapidly injected with a syringe in a fume hood.

[0018] According to a further technical solution, in step 5, the medicine is weighed in a glove box and placed in a three-necked flask, and the flask mouth is sealed with a rubber stopper.

[0019] According to a further technical solution, the centrifugation time in step 8 is 5 minutes.

[0020] According to a further technical solution, the drying temperature in step 9 is 60° C. and the drying time is 6 hours.

[0021] Another object of an embodiment of the present invention is to provide a method for preparing a three-dimensional semiconductor GaN nanoflower material, wherein the reaction time of the above step 7 is adjusted to 30s, 1min, 10min, 15min, 30min, 1h, 2h, 3h and 4h, respectively, and the other steps remain unchanged, to obtain GaN-30s, GaN-1min, GaN-10min, GaN-15min, GaN-30min, GaN-1h, GaN-2h, GaN-3h and GaN-4h, respectively.

[0022] The embodiment of the present invention provides a method for preparing a three-dimensional semiconductor GaN nanoflower material, which uses a solvothermal method to synthesize a three-dimensional tunable GaN nanoflower material with a stable crystal structure, low sample cost, and environmental friendliness, and obtains a tunable GaN nanoflower material by controlling the reaction time. The obtained three-dimensional GaN nanoflower has a large specific surface area and abundant active sites. In addition, the GaN nanoflower material increases the specific surface area, improves the electron transport performance, enhances the catalytic performance, and enhances the light absorption performance, showing more significant performance advantages in the fields of photocatalysis, electrocatalysis, gas sensors, and optoelectronic devices. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 is the X-ray diffraction (XRD) pattern of each sample;

[0024] Figure 2 is the Fourier transform infrared spectrum (FT-IR) of each sample;

[0025] Figure 3 is a scanning electron microscope (SEM) image of GaN-3h;

[0026] Figure 4 TEM image of GaN-3h;

[0027] Figure 5 This is the energy spectrum analysis (EDS) image of GaN-3h;

[0028] Figure 6 X-ray photoelectron spectroscopy (XPS) of Ga 3d and N1s of GaN-3h and GaN-15min. DETAILED DESCRIPTION

[0029] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0030] The specific implementation of the present invention is described in detail below in conjunction with specific embodiments.

[0031] An embodiment of the present invention provides a method for preparing a three-dimensional semiconductor GaN nanoflower material, comprising the following steps:

[0032] Step 1: Pour 2 ml of octadecene into a three-necked flask, connect the system, and degas for 15 min at room temperature;

[0033] Step 2: Raise the reaction temperature to 120°C, degas for 20 min, and then cool down to 60°C in a N2 atmosphere;

[0034] Step 3: Rapidly inject 2 ml of lithium bis(trimethylsilyl)amide and degas at room temperature for at least 20 min;

[0035] Step 4: degassing at 120 °C for 20 min under N2 atmosphere, cooling to 60 °C to obtain a ligand solution;

[0036] Step 5: 88 mg of gallium chloride, 0.478 ml of oleylamine and 5 ml of octadecene were placed in a three-necked flask;

[0037] Step 6: After degassing at 120°C for 15 min, the temperature was raised to 320°C in a N2 atmosphere;

[0038] Step 7: Rapidly inject 1.5 ml of the ligand solution in step 6, and react for 15 seconds to obtain GaN-15s;

[0039] Step 8: The obtained solution was washed with n-hexane, methanol, ethanol and acetone respectively and centrifuged;

[0040] Step 9: Place the powder obtained after washing in a vacuum drying oven for drying to obtain a three-dimensional GaN-15s nanoflower product.

[0041] As a preferred embodiment of the present invention, in the step 1, octadecene is 1-Octadecene, which is injected into a three-necked flask using a pipette.

[0042] As a preferred embodiment of the present invention, in step 1 and step 5, a magnet is added into the three-necked flask, and the rotation speed of the magnet in the solution is 660 rpm.

[0043] As a preferred embodiment of the present invention, in step 3, a lithium bis(trimethylsilyl)amide solution (5.32 mol / L) is rapidly injected into the fume hood using a syringe.

[0044] As a preferred embodiment of the present invention, in step 5, the medicine is weighed in a glove box and placed in a three-necked flask, and the flask mouth is sealed with a rubber stopper.

[0045] As a preferred embodiment of the present invention, the centrifugation time in step 8 is 5 minutes.

[0046] As a preferred embodiment of the present invention, the drying temperature in step 9 is 60° C. and the drying time is 6 hours.

[0047] Another embodiment of the present invention provides a method for preparing a three-dimensional semiconductor GaN nanoflower material, wherein the reaction time of the above step 7 is adjusted to 30s, 1min, 10min, 15min, 30min, 1h, 2h, 3h and 4h, respectively, and the other steps remain unchanged, to obtain GaN-30s, GaN-1min, GaN-10min, GaN-15min, GaN-30min, GaN-1h, GaN-2h, GaN-3h and GaN-4h, respectively.

[0048] The X-ray diffraction (XRD) patterns of the prepared GaN-15s, GaN-30s, GaN-1min, GaN-10min, GaN-15min, GaN-30min, GaN-1h, GaN-2h, GaN-3h and GaN-4h are as follows: Figure 1 As shown in the figure, the characteristic peaks of the ten GaN samples obtained correspond to the GaN standard card (PDF#50-0792). In addition, as the reaction time increases, the diffraction characteristic peaks of the samples gradually increase, indicating that the crystallinity of the GaN material is better. The Fourier transform infrared spectra (FT-IR) of the above samples are shown in the figure. Figure 2 As shown, the test results show that the surface of the semiconductor material is located at 3434cm -1 、2925cm -1 、1263cm -1 and 957cm -1 The characteristic peaks nearby correspond to functional groups such as -OH, CH, CC and Si-O.

[0049] Among them, the scanning electron microscope (SEM) image of GaN-3h is as follows Figure 3 As shown in the figure, it can be seen that the sample presents a uniform three-dimensional flower-like morphology with a size of about 200nm. The TEM image of GaN-3h is shown in Figure 4 As shown in the figure, it can be seen that the sample is aggregated into a three-dimensional nanoflower structure by nanosheets. The energy spectrum analysis (EDS) image of GaN-3h is shown in Figure 5 As shown in the figure, it can be seen that Ga, N, Si, O and C elements are evenly dispersed on the surface of the sample.

[0050] The X-ray photoelectron spectroscopy (XPS) of Ga 3d and N1s of GaN-3h and GaN-15min is shown in Figure 2. Figure 6 As shown, from the test results, it can be seen that N-Ga exists on the surface of the material, which further confirms the successful preparation of GaN material.

[0051] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a three-dimensional semiconductor GaN nanoflower material, characterized in that: The following steps are involved: Step 1: Pour 2 ml of octadecene into a three-necked flask, connect the system, and degas for 15 min at room temperature; Step 2: Raise the reaction temperature to 120°C, degas for 20 min, and then cool down to 60°C in a N2 atmosphere; Step 3: Rapidly inject 2 ml of lithium bis(trimethylsilyl)amide and degas at room temperature for at least 20 min; Step 4: degassing at 120 °C for 20 min under N2 atmosphere, cooling to 60 °C to obtain a ligand solution; Step 5: 88 mg of gallium chloride, 0.478 ml of oleylamine and 5 ml of octadecene were placed in a three-necked flask; Step 6: After degassing at 120°C for 15 min, the temperature was raised to 320°C in a N2 atmosphere; Step 7: Rapidly inject 1.5 ml of the ligand solution in step 6, and react for 15 seconds to obtain GaN-15s; Step 8: The obtained solution was washed with n-hexane, methanol, ethanol and acetone respectively and centrifuged; Step 9: Place the powder obtained after washing in a vacuum drying oven for drying to obtain a three-dimensional GaN-15s nanoflower product.

2. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 1, characterized in that: In the step 1, octadecene is 1-Octadecene, which is injected into a three-necked flask using a pipette.

3. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 2, characterized in that: In step 1 and step 5, a magnet is added into the three-necked flask, and the rotation speed of the magnet in the solution is 660 rpm.

4. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 2, characterized in that: In step 3, the lithium bis(trimethylsilyl)amide solution is rapidly injected into the mixture using a syringe in a fume hood.

5. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 2, characterized in that: In step 5, the drug is weighed in a glove box and placed in a three-necked flask, and the flask mouth is sealed with a rubber stopper.

6. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 2, characterized in that: The centrifugation time in step 8 is 5 min.

7. The method for preparing the three-dimensional semiconductor GaN nanoflower material according to claim 2, characterized in that: The drying temperature in step 9 is 60° C. and the drying time is 6 hours.

8. A method for preparing a three-dimensional semiconductor GaN nanoflower material, based on the method for preparing a three-dimensional semiconductor GaN nanoflower material according to any one of claims 1 to 7, characterized in that: The reaction time of the above step 7 was adjusted to 30s, 1min, 10min, 15min, 30min, 1h, 2h, 3h and 4h, respectively, and the other steps remained unchanged. The obtained products were named GaN-30s, GaN-1min, GaN-10min, GaN-15min, GaN-30min, GaN-1h, GaN-2h, GaN-3h and GaN-4h, respectively.

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