CN112850664A - Preparation method of gallium nitride nanosheet - Google Patents

Preparation method of gallium nitride nanosheet Download PDF

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CN112850664A
CN112850664A CN202110105234.2A CN202110105234A CN112850664A CN 112850664 A CN112850664 A CN 112850664A CN 202110105234 A CN202110105234 A CN 202110105234A CN 112850664 A CN112850664 A CN 112850664A
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李恩玲
刘畅
赵宏远
郑艳鹏
沈鹏飞
白凯飞
崔真
马德明
张琳
沈洋
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Xian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

The invention discloses a preparation method of gallium nitride nanosheets, which comprises the following specific steps: step 1: adding solid GaCl3Dissolving in deionized water to obtain a certain amount of GaCl3Adding the solution into a beaker, and then sequentially adding a certain amount of hydrochloric acid solution, urea, oxalic acid dihydrate and polyvinylpyrrolidone into the beaker; step 2: transferring the solution obtained in the step (1) into a reaction kettle lining, then placing the reaction kettle lining containing the solution into a heating furnace for heat treatment, and cleaning the obtained product with deionized water and absolute ethyl alcohol to obtain a precipitate; and step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets; and 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheets andNH3and (4) carrying out reaction to prepare the GaN nanosheet. The method has the advantages of simple process, simple experimental equipment, low cost, good benefit and easy realization of commercialization.

Description

Preparation method of gallium nitride nanosheet
Technical Field
The invention belongs to the technical field of nano material preparation methods, and particularly relates to a preparation method of gallium nitride nanosheets.
Background
Gallium nitride (GaN) is currently the hotspot and leading edge of global semiconductor research as a third-generation semiconductor material, and as a typical two-dimensional layered semiconductor, the successful preparation of GaN nanosheets can provide a solid foundation for the design and preparation of electronic devices, and further promote the application of electronic devices. GaN is chemically stable and has many excellent physical properties including a wide band gap, a small dielectric constant, a high breakdown voltage, a high thermal conductivity, etc., so that it has a wide application prospect in the fields of optoelectronic devices and functional devices. According to the existing reports, GaN is widely applied to blue LEDs and also applied to the fields of high-power devices and aerospace. In recent years, with the advent of hot trends in graphene research, a large number of two-dimensional materials have attracted attention from researchers. The structure of two-dimensional GaN is similar to graphene, and is a hexagonal honeycomb structure having a planar structure. As the dimension decreases, the physical properties thereof also significantly change, including electronic and optical properties, and the band gap of two-dimensional GaN has been reported to exceed 4 eV. In order to apply two-dimensional GaN to practice, a GaN nanosheet structure with a good appearance must be prepared, which attracts a great number of researchers to compete for research, and some experimental methods including a Chemical Vapor Deposition (CVD) method, a packaging migration method, a template method and the like are reported at present. However, these methods have some problems, for example, it is difficult to ensure the morphology of the deposited GaN nanosheet by the CVD method, and the requirement of the package migration method is very high.
Disclosure of Invention
The invention aims to provide a preparation method of gallium nitride nanosheets, which can be used for preparing GaN nanosheet materials with good appearances and uniform texture.
The technical scheme adopted by the invention is that the preparation method of the gallium nitride nanosheet comprises the following specific steps:
step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into the beaker, and stirring for 25-40 minutes to obtain solution A;
step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
and step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
and 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3And (4) carrying out reaction to prepare the GaN nanosheet.
The present invention is also characterized in that,
in step 1, GaCl was used3The concentration of the solution is 0.1-0.2mol/L, and the concentration of the hydrochloric acid solution is 0.3-0.4mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1: 4-5, and PVP-K30 and OAD are added to the solution, and Ga in the solution3+The amount of the substance(s) is kept at 1:2 to 3:1, and the pH value of the solution A after the reaction is controlled by urea to be 6.8 to 7.9.
In the step 2, the heat treatment process specifically comprises the following steps: the reaction kettle is heated to the temperature of 220 ℃ and 260 ℃ and then is kept for 3-5 h.
In step 3, the precipitate obtained in step 2 is dried for 12-18h at the temperature of 60-80 ℃.
In step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tubular furnace is controlled at 800-900 ℃ and NH3The flow rate is 100-.
The invention has the beneficial effects that: the method uses GaCl3Preparing Ga from solution, hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD), polyvinylpyrrolidone (PVP-K30) and other substances by hydrothermal method under specific process conditions2O3Nanosheets, and Ga2O3Nanosheet and NH3Reacting to prepare a GaN nanosheet material with good appearance and uniform texture; the preparation method has the advantages of simple process, simple experimental equipment, low cost, good benefit and easy realization of commercialization.
Drawings
FIG. 1 is a view showing Ga prepared in example 1 of the present invention2O3SEM image of 4 ten thousand times of magnification of the nano sheet;
FIG. 2 shows Ga prepared in example 1 of the present invention2O3XRD images of the nanosheets;
FIG. 3 is an SEM image of GaN nanosheets prepared in example 1 of the present invention at a magnification of 4 ten thousand times;
FIG. 4 is an XRD image of GaN nanosheets prepared in example 1 of the present invention;
fig. 5 is an EDS image of GaN nanosheets prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of gallium nitride nanosheets, which comprises the following specific steps:
step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, and sequentially adding a certain amount of the solutionAdding hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into a beaker, and stirring for 25-40 minutes to obtain solution A;
in step 1, GaCl was used3The concentration of the solution is 0.1-0.2mol/L, and the concentration of the hydrochloric acid solution is 0.3-0.4mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1: 4-5, and PVP-K30 and OAD are added to the solution, and Ga in the solution3+The amount of the substance(s) is kept at 1:2 to 3:1, and the pH value of the solution A after the reaction is controlled by urea to be 6.8 to 7.9.
Step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
in the step 2, the heat treatment process specifically comprises the following steps: the reaction kettle is heated to the temperature of 220 ℃ and 260 ℃ and then is kept for 3-5 h.
And step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
in step 3, the precipitate obtained in step 2 is dried for 12-18h at the temperature of 60-80 ℃.
And 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3Carrying out reaction to prepare GaN nanosheets;
in step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tubular furnace is controlled at 800-900 ℃ and NH3The flow rate is 100-.
Example 1
Using GaCl3Solution, hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) are synthesized into Ga by a hydrothermal method2O3Nanosheets.
5ml of GaCl with the concentration of 0.14mol/L are respectively measured by a measuring cylinder3The solution and 25ml of 0.4mol/L hydrochloric acid solution are prepared by electron beam irradiation0.5g of urea, 0.265g of oxalic acid dihydrate and 78mg of polyvinylpyrrolidone (PVP-K30) are weighed in a flat manner, the raw materials are poured into a beaker of 50ml, stirred for 30min by a magnetic stirrer, the pH value of the solution is controlled by the urea, the pH value of the solution after the reaction is kept at 7, and the solution is moved into a reaction kettle lining after being completely dissolved and is placed in a heating furnace. Setting the temperature of a heating furnace at 230 ℃, heating the heating furnace to the set temperature, keeping for 4 hours, after the hydrothermal reaction is finished, naturally cooling to room temperature, washing the obtained product for 4 times by using deionized water and absolute ethyl alcohol, filtering, and drying the obtained precipitate for 12 hours at 80 ℃ to obtain Ga2O3Nanosheets.
Ga is mixed with2O3The nano-sheets are uniformly dispersed in a quartz boat and then placed in a tube furnace, the temperature of the heating furnace is set to 850 ℃, and in the temperature rising process, argon is used as a protective gas to avoid oxygen entering the tube to influence the reaction. When the heating furnace is heated to the set temperature, the argon is closed, and NH with the ventilation flow of 100sccm3The reaction time is 30min, and NH is closed after the reaction time reaches the set time3Then argon is introduced, and finally the GaN nanosheet is naturally cooled to room temperature, so that the preparation of the GaN nanosheet is completed.
This example uses GaCl3Solution, hydrochloric acid solution, urea, oxalic acid dihydrate and polyvinylpyrrolidone (PVP-K30) are used as raw materials, and Ga is synthesized by a hydrothermal method2O3Nanosheets, SEM results (as shown in FIG. 1) indicate Ga2O3The nano material is nano-sheet in shape, and is uniform in distribution and good in shape. For prepared Ga2O3XRD testing of the sample revealed (as shown in FIG. 2) that Ga was present in the sample2O3In the standard XRD card comparison (JCPDS 20-0426), no impurity peak is detected in the structure, and all diffraction peaks are attributed to gamma-Ga in a face-centered cubic structure2O3And (5) structure.
In this example, XRD patterns of GaN nanosheets were prepared, as shown in fig. 4. The peak values (100), (002), (101), (102), (110), (103), (112), (201) of the crystal planes are consistent with the standard XRD card of wurtzite GaN. The structure can be seen through XRD testGaN prepared under this condition is already Ga-free2O3Proves Ga under these conditions2O3The nanosheet template is completely aminated, and an XRD (X-ray diffraction) pattern shows that the nanosheet template is free of a miscellaneous peak, and the GaN nanosheet sample prepared under the condition is high in purity.
As shown in fig. 3, the prepared GaN nanosheets are uniformly distributed; FIG. 5 and Table 1 show the analysis of the EDS composition of GaN nanosheets produced in this example. The test result totally contains C, O, Ga, N and Cu elements. C and O in the EDS results are mainly due to their low peak energy ratio, and their element ratios are detected, thus having no influence on the results, while the Cu ratios are mainly due to the Cu substrate used in the test. From the EDS test results, the Ga and N contents remained roughly 1:1, which also demonstrates that the reactant under this condition is GaN.
TABLE 1
Figure BDA0002917132580000061
Example 2
Step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into the beaker, and stirring for 25 minutes to obtain a solution A;
in step 1, GaCl was used3The concentration of the solution is 0.1mol/L, and the concentration of the hydrochloric acid solution is 0.3mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1:4, and PVP-K30, OAD and Ga in the solution are added3+The amount of substance (b) was kept at 1:2:1, and the pH of the solution a after completion of the reaction was kept at 6.8 by controlling the pH of the solution with urea.
Step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
in the step 2, the heat treatment process specifically comprises the following steps: the autoclave was heated to 220 ℃ and then held for 3 h.
And step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
in step 3, the precipitate obtained in step 2 is dried for 12h at the temperature of 60-80 ℃.
And 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3Carrying out reaction to prepare GaN nanosheets;
in step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tube furnace was controlled at 800 ℃ and NH3The flow rate was 100sccm and the reaction time was 20 min.
Example 3
Step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into the beaker, and stirring for 40 minutes to obtain a solution A;
in step 1, GaCl was used3The concentration of the solution is 0.2mol/L, and the concentration of the hydrochloric acid solution is 0.4mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1:5, and PVP-K30, OAD and Ga in the solution are added3+The amount of substance (b) was maintained at 1:3:1, and the pH of the solution a after completion of the reaction was maintained at 7.9 by controlling the pH of the solution with urea.
Step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
in the step 2, the heat treatment process specifically comprises the following steps: the autoclave was heated to 260 ℃ and then held for 5 h.
And step 3: drying the precipitate obtained in the step 2Drying to obtain Ga2O3Nanosheets;
in step 3, the precipitate obtained in step 2 is dried for 18h at the temperature of 60-80 ℃.
And 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3Carrying out reaction to prepare GaN nanosheets;
in step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tube furnace was controlled at 900 ℃ and NH3The flow rate was 150sccm and the reaction time was 40 min.
Example 4
Step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into the beaker, and stirring for 30 minutes to obtain a solution A;
in step 1, GaCl was used3The concentration of the solution is 0.15mol/L, and the concentration of the hydrochloric acid solution is 0.35mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1:4.5, and PVP-K30 and OAD are added to the solution and Ga in the solution3+The amount of substance (b) was maintained at 1:2.5:1, and the pH of the solution a after completion of the reaction was maintained at 7 by controlling the pH of the solution with urea.
Step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
in the step 2, the heat treatment process specifically comprises the following steps: the autoclave was heated to 250 ℃ and then held for 4 h.
And step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
in step 3, the precipitate obtained in step 2 is dried for 15h at the temperature of 60-80 ℃.
And 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3Carrying out reaction to prepare GaN nanosheets;
in step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tube furnace was controlled at 850 ℃ and NH3The flow rate was 120sccm and the reaction time was 30 min.
Example 5
Step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, Oxalic Acid Dihydrate (OAD) and polyvinylpyrrolidone (PVP-K30) into the beaker, and stirring for 50 minutes to obtain a solution A;
in step 1, GaCl was used3The concentration of the solution is 0.1mol/L, and the concentration of the hydrochloric acid solution is 0.4mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1:5, and PVP-K30, OAD and Ga in the solution are added3+The amount of substance (b) was maintained at 1:2:1, and the pH of the solution a after completion of the reaction was maintained at 7.9 by controlling the pH of the solution with urea.
Step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
in the step 2, the heat treatment process specifically comprises the following steps: the autoclave was heated to 220 ℃ and then held for 5 h.
And step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
in step 3, the precipitate obtained in step 2 is dried for 18h at the temperature of 60-80 ℃.
And 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3The reaction is carried out, and the reaction solution is mixed,preparing GaN nanosheets;
in step 4, certain reaction conditions in the tube furnace are as follows: the reaction temperature in the tube furnace was controlled at 800 ℃ and NH3The flow rate was 100sccm and the reaction time was 40 min.
The invention synthesizes Ga by a hydrothermal method2O3Nanosheet as template, Ga2O3The template is reacted with NH in a tube furnace under optimum process conditions3The reaction is carried out to prepare pure high-quality GaN nanosheets with hexagonal crystal structures, and the method is simple and convenient, has low requirements on equipment and has potential application value.

Claims (5)

1. A preparation method of gallium nitride nanosheets is characterized by comprising the following specific steps:
step 1: adding solid GaCl3Dissolving in deionized water to obtain GaCl3Taking a certain amount of GaCl3Adding the solution into a beaker, then sequentially adding a certain amount of hydrochloric acid solution, urea, oxalic acid dihydrate and polyvinylpyrrolidone into the beaker, and stirring for 25-40 minutes to obtain a solution A;
step 2: transferring the solution A obtained in the step 1 into a reaction kettle lining, then placing the reaction kettle lining containing the solution A into a heating furnace for heat treatment, naturally cooling to room temperature after the heat treatment, cleaning the obtained product with deionized water and absolute ethyl alcohol, and filtering to obtain a precipitate;
and step 3: drying the precipitate obtained in the step 2 to obtain Ga2O3Nanosheets;
and 4, step 4: ga is mixed with2O3Placing the nano-sheets into a quartz boat, placing the quartz boat into a tube furnace, and under certain reaction conditions, placing Ga into the tube furnace2O3Nanosheet and NH3And (4) carrying out reaction to prepare the GaN nanosheet.
2. A process for preparing gallium nitride nanosheets according to claim 1, wherein in step 1 GaCl is used3The concentration of the solution is 0.1-0.2mol/L, and the concentration of the hydrochloric acid solution is 0.3-0.4mol/L, GaCl3The volume ratio of the solution to the hydrochloric acid solution is 1: 4-5, and PVP-K30 and OAD are added to the solution, and Ga in the solution3+The amount of the substance(s) is kept at 1:2 to 3:1, and the pH value of the solution A after the reaction is controlled by urea to be 6.8 to 7.9.
3. The method for preparing gallium nitride nanosheets according to claim 1, wherein in step 2, the heat treatment process specifically comprises: the reaction kettle is heated to the temperature of 220 ℃ and 260 ℃ and then is kept for 3-5 h.
4. A method for preparing gallium nitride nanosheets according to claim 1, wherein in step 3, the precipitate obtained in step 2 is dried at 60-80 ℃ for 12-18 h.
5. A method for preparing gallium nitride nanosheets according to claim 1, wherein in step 4, certain reaction conditions in the tube furnace are specifically: the reaction temperature in the tubular furnace is controlled at 800-900 ℃ and NH3The flow rate is 100-.
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Application publication date: 20210528