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CN111204719A - Gallium nitride nanotube and preparation method thereof - Google Patents

Gallium nitride nanotube and preparation method thereof Download PDF

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CN111204719A
CN111204719A CN202010133005.7A CN202010133005A CN111204719A CN 111204719 A CN111204719 A CN 111204719A CN 202010133005 A CN202010133005 A CN 202010133005A CN 111204719 A CN111204719 A CN 111204719A
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gallium nitride
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zinc oxide
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季小红
曹发
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South China University of Technology SCUT
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    • C01B21/00Nitrogen; Compounds thereof
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    • C01B21/0632Binary 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
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Abstract

本发明公开了一种氮化镓纳米管及其制备方法,属于形貌控制材料制备领域。所述方法包括:(1)将衬底进行表面预处理,采用直流磁控溅射法在衬底的表面溅射一层氧化锌缓冲层;(2)将衬底放置在装有反应溶液的反应釜中,水热反应生成氧化锌纳米棒。(3)把长有氧化锌纳米棒的衬底放在原子束沉积腔体中沉积氮化镓壳层。(4)用移液枪量取适量配置好的硫酸溶液滴在长有氧化锌/氮化镓核壳层的衬底上,使硫酸溶液充分腐蚀氧化锌纳米棒,最后在衬底上留下氮化镓纳米管。本发明实现了氮化镓纳米管的可控制备,且制备方法简单、重复性好、质量可靠。

Figure 202010133005

The invention discloses a gallium nitride nanotube and a preparation method thereof, belonging to the field of shape control material preparation. The method includes: (1) performing surface pretreatment on the substrate, and sputtering a zinc oxide buffer layer on the surface of the substrate by using a DC magnetron sputtering method; (2) placing the substrate in a reaction solution In the reactor, the hydrothermal reaction generates zinc oxide nanorods. (3) The gallium nitride shell layer is deposited by placing the substrate with ZnO nanorods in the atomic beam deposition chamber. (4) Use a pipette to measure an appropriate amount of the prepared sulfuric acid solution and drop it on the substrate with the zinc oxide/gallium nitride core-shell layer, so that the sulfuric acid solution can fully corrode the zinc oxide nanorods, and finally leave on the substrate. Gallium Nitride Nanotubes. The invention realizes the controllable preparation of the gallium nitride nanotube, and has the advantages of simple preparation method, good repeatability and reliable quality.

Figure 202010133005

Description

Gallium nitride nanotube and preparation method thereof
Technical Field
The invention belongs to the field of preparation of morphology control materials, and particularly relates to a gallium nitride nanotube and a preparation method thereof.
Background
Due to the size and the shape of the one-dimensional nano structure and excellent electric, optical and magnetic properties, the one-dimensional nano structure is widely applied to the fields of optics, electromagnetism, catalysis, biological detection, drug transportation and the like. The direct band gap wide band gap semiconductor gallium nitride (the band gap width is 3.4eV) is a typical representative of the third generation wide band gap semiconductor. Gallium nitride has many excellent characteristics such as large electron mobility, good electric and thermal conductivity, high breakdown field strength, high temperature resistance, corrosion resistance, good radiation resistance and the like. In addition, the material has a great application prospect in ultraviolet and blue light LED devices and ultraviolet detection devices, and is one of the most excellent materials for manufacturing high-power photoelectric devices.
At present, the preparation methods of the gallium nitride nano material are infinite, including chemical vapor deposition, metal organic chemical vapor deposition and pulsed laser deposition, and the preparation methods have the defect that the preparation methods all need higher temperature; the prepared gallium nitride nanometer material has the appearance including a nanometer rod, a nanometer tower, a nanometer wire and the like, but few literature reports about the preparation method of the gallium nitride nanometer tube exist, Jiangshuai and the like in a patent (application publication No. CN 104419982A) mention that the gallium nitride nanometer tube is prepared by a zinc oxide template through a chemical vapor deposition method at high temperature, but the preparation temperature is too high (850-. Therefore, it is very important to find a method for preparing the gallium nitride nanotube at low temperature.
The gallium nitride nanotube not only has the unique photoelectric and physicochemical characteristics of the gallium nitride nanomaterial, but also can be uniquely applied to the fields of photoelectric devices, catalysis, biological detection and the like due to the unique tubular structure. How to find a simple and controllable method for preparing the gallium nitride nanotube is the premise for realizing the application of the gallium nitride nanotube.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a gallium nitride nanotube and a preparation method thereof.
The invention aims to provide a preparation method of a gallium nitride nanotube, which is characterized in that a zinc oxide nanorod is used as a template, then an atomic beam is used for depositing a gallium nitride nanosheet layer, and the template is removed through acid corrosion to prepare the gallium nitride nanotube. The inner diameter, the outer diameter and the length of the gallium nitride nanotube can be controllably prepared by controlling the diameter and the length of the zinc oxide nanorod and the number of turns of gallium nitride deposited by an atomic beam; the method has good repeatability and reliable quality in the process of preparing the gallium nitride nanotube and is easy for large-scale production.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a gallium nitride nanotube, which comprises the following steps:
(1) ultrasonically cleaning the substrate for 10-15min by alcohol and deionized water respectively, drying the substrate by blowing nitrogen, and sputtering a zinc oxide buffer layer with the thickness of 80-120nm on the silicon substrate by adopting a direct-current magnetron sputtering method (the sputtering condition is that the power is 80W, the time is 150-200s, the argon gas is 12sccm, and the pressure is 0.3 Pa);
(2) placing the substrate sputtered with the buffer layer in a reaction kettle filled with reaction solution (70 ml; 0.02-0.03M zinc nitrate, 0.02-0.03M hexamethylenetetramine, and the molar ratio is 1: 1), carrying out hydrothermal reaction at 90-95 ℃ for 5-8h, taking out, washing with deionized water, and drying at 60-80 ℃ for 5-10 min;
(3) and placing the substrate with the zinc oxide nanorods in an atomic beam deposition cavity to deposit a gallium nitride shell layer. The precursor is triethyl gallium (99.99 percent) and hydrogen-nitrogen mixed gas (the volume ratio is 1/4), the reaction temperature is 200-300 ℃, the plasma power is 200w, and the cycle times are 300-400. The method comprises the following specific steps: the pulse time of the triethyl gallium is 0.03-0.04s, the reaction time is 10-15s, the cleaning time is 40-60s, the plasma time of the nitrogen-hydrogen mixed gas is 10-20s, the cleaning is carried out for 40-60s again, and the steps are repeated for 400 times.
(4) Dropping a proper amount of prepared dilute sulfuric acid solution (100ml of water +1-3 drops of concentrated sulfuric acid) on the substrate with the zinc oxide/gallium nitride core shell growing thereon by using a liquid transfer gun, reacting for 5-10min, heating the substrate to 50-70 ℃, drying the dilute sulfuric acid solution, repeating for 2-3 times, dropping deionized water to wash impurity ions remained on the surface, and drying at 60-80 ℃.
Further, the substrate in the step (1) is one of a silicon substrate, a silicon dioxide substrate and an aluminum oxide substrate.
Further, the thickness of the zinc oxide in the step (1) is 80-120 nm.
Further, in the mixed solution of zinc nitrate and hexamethylenetetramine in the step (2), the concentration of zinc nitrate is 0.02-0.03M, and the concentration of hexamethylenetetramine is 0.02-0.03M.
Further, in the mixed solution of zinc nitrate and hexamethylenetetramine in the step (2), the molar ratio of zinc nitrate to hexamethylenetetramine is 1: 1.
Further, the temperature of the hydrothermal reaction in the step (2) is 90-95 ℃, the time of the hydrothermal reaction is 5-8h, the drying temperature is 60-80 ℃, and the drying time is 5-10 min.
Further, in the step (3), the reaction temperature for depositing the gallium nitride shell is 200-300 ℃, and the atmosphere for depositing the gallium nitride shell is the mixed atmosphere of hydrogen and nitrogen; the volume ratio of the hydrogen to the nitrogen is 1: 4.
further, in the step (3), the step of depositing the gallium nitride shell layer comprises: the triethyl gallium is pulsed for 0.03-0.04s, the reaction time is 10-15s, the cleaning time is 40-60s, the plasma time of the mixed atmosphere of nitrogen and hydrogen is 10-20s, cleaning is carried out again for 40-60s, and the steps are repeated for 400 times.
Further, the pH value of the dilute sulfuric acid solution in the step (4) is 1.5-4; the standing reaction time is 5-10 min; the temperature for heating and drying is 50-70 ℃.
The invention provides a gallium nitride nanotube prepared by the preparation method.
The preparation method of the gallium nitride nanotube provided by the invention is characterized in that the diameter and the length of the zinc oxide template are regulated and controlled by a hydrothermal method, and the number of atomic beam deposition turns is changed, so that the controllable preparation of the length, the inner diameter and the outer diameter of the gallium nitride nanotube is realized, the repeatability is good, the quality is reliable, and the large-scale preparation of the gallium nitride nanotube material can be realized.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method of the gallium nitride nanotube, the length and the diameter of the nanorod are controlled by a hydrothermal method, so that the controllable preparation of the length and the inner diameter of the gallium nitride nanotube can be realized;
(2) according to the preparation method of the gallium nitride nanotube, the controllable preparation of the wall thickness of the gallium nitride nanotube can be realized through the number of atomic beam deposition layers;
(3) the preparation method of the gallium nitride nanotube provided by the invention can be used for preparing the gallium nitride nanotube at low temperature.
Drawings
FIG. 1 is a schematic diagram of a process for preparing GaN nanotubes according to an embodiment of the invention;
the structure comprises a silicon layer 1, a zinc oxide buffer layer 2, a zinc oxide nanorod 3, a zinc oxide/gallium nitride core shell 4 and a gallium nitride nanotube 5, wherein the zinc oxide/gallium nitride core shell is formed by a silicon nitride layer and a zinc oxide/gallium nitride core shell;
FIG. 2 is a scanning electron micrograph of the zinc oxide nanorods prepared in example 1;
FIG. 3 is an X-ray diffraction pattern of gallium nitride nanotubes prepared in example 1;
FIG. 4 is a scanning electron micrograph of the GaN nanotubes prepared in example 1.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
In the embodiment, a specific process schematic diagram for preparing a gallium nitride nanotube can be shown in fig. 1, wherein a silicon layer 1, a zinc oxide buffer layer 2, a zinc oxide nanorod 3, a zinc oxide/gallium nitride core shell 4, and a gallium nitride nanotube 5 are provided.
The atomic beam deposition equipment model is as follows: jiaxing Kemin PEALD-100R.
Example 1
(1) Magnetron sputtering: ultrasonically cleaning a silicon substrate (a silicon layer 1) for 15min by alcohol and deionized water respectively, drying the silicon substrate by using nitrogen, and carrying out magnetron sputtering on the silicon substrate by using a direct-current magnetron sputtering method (the sputtering conditions are that the power is 80W, the time is 150s, the argon flow is 12sccm, and the pressure is 0.3Pa) to form a zinc oxide buffer layer 2 with the thickness of 80 nm;
(2) hydrothermal method: the substrate sputtered with the buffer layer is placed in a reaction kettle filled with reaction solution (70 ml; 0.02M zinc nitrate, 0.02M hexamethylenetetramine), hydrothermal reaction is carried out for 5h at 95 ℃, then the substrate is taken out, washed by deionized water and dried for 5min at 80 ℃ to obtain the zinc oxide nano rod 3, as shown in figure 2, the diameter of the nano rod is relatively uniform and is about 200 nm.
(3) Atomic beam deposition: and (3) placing the substrate with the zinc oxide nanorods in an atomic beam deposition cavity to deposit a gallium nitride shell layer to obtain the zinc oxide/gallium nitride core shell 4. The precursor is triethyl gallium (99.99 percent) and hydrogen-nitrogen mixed gas (the volume ratio is 1/4), the reaction temperature is 200 ℃, the plasma power is 200w, and the cycle number is 400 times. The method comprises the following specific steps: the pulse time of the triethyl gallium is 0.03s, the reaction time is 10s, the cleaning time is 40s, the plasma time of the nitrogen-hydrogen mixed gas is 10s, the cleaning is carried out for 40s again, and the steps are repeated for 400 times.
(4) Acid corrosion: and (2) dropping 300 mu l of prepared dilute sulfuric acid solution (100ml of water +3 drops of concentrated sulfuric acid, the pH value is 1.5) on the substrate with the zinc oxide/gallium nitride core shell, reacting for 5min, heating the substrate to 60 ℃, drying the dilute sulfuric acid solution, repeating for 3 times, dropping deionized water to wash residual impurity ions on the surface, and drying at 80 ℃ to obtain the gallium nitride nanotube 5.
FIG. 3 is an x-ray diffraction pattern of the prepared nanotubes, wherein the diffraction peaks can be assigned to the (100), (101), (110) and (112) peaks of gallium nitride (PDF #88-2631), respectively. FIG. 4 shows that the prepared GaN nano material has a tubular structure by scanning electron microscopy, and the inner diameter of the GaN nano material is the diameter of the zinc oxide nano rod and is about 200 nm. In conclusion, the gallium nitride nanotube is successfully and controllably prepared by the method.
Example 2
(1) Ultrasonically cleaning a silicon dioxide substrate for 15min by alcohol and deionized water respectively, drying the silicon dioxide substrate by blowing nitrogen, and sputtering a zinc oxide buffer layer with the thickness of 80nm on the silicon substrate by adopting a direct-current magnetron sputtering method (the sputtering condition is that the power is 80W, the time is 150s, the argon flow is 12sccm, and the pressure is 0.3 Pa);
(2) the substrate sputtered with the buffer layer is placed in a reaction kettle filled with reaction solution (70 ml; 0.02M zinc nitrate, 0.02M hexamethylenetetramine), hydrothermal reaction is carried out for 5h at 95 ℃, then the substrate is taken out, washing is carried out by deionized water, and drying is carried out for 5min at 80 ℃ to obtain the zinc oxide nano-rod, wherein the diameter of the nano-rod is relatively uniform and is about 200 nm.
(3) And placing the substrate with the zinc oxide nanorods in an atomic beam deposition cavity to deposit a gallium nitride shell layer. The precursor is triethyl gallium (99.99 percent) and hydrogen-nitrogen mixed gas (the volume ratio is 1/4), the reaction temperature is 200 ℃, the plasma power is 200w, and the cycle number is 400 times. The method comprises the following specific steps: the pulse time of the triethyl gallium is 0.04s, the reaction time is 10s, the cleaning time is 40s, the plasma time of the nitrogen-hydrogen mixed gas is 10s, the cleaning is carried out for 40s again, and the steps are repeated for 400 times.
(4) And (2) dropping 300 mu l of prepared dilute sulfuric acid solution (100ml of water +3 drops of concentrated sulfuric acid, ph-1.5) on the substrate with the zinc oxide/gallium nitride core shell, reacting for 5min, heating the substrate to 60 ℃, drying the dilute sulfuric acid solution, repeating for 3 times, dropping deionized water to wash impurity ions remained on the surface, and drying at 80 ℃ to obtain the gallium nitride nanotube.
Example 3
(1) Ultrasonically cleaning a silicon substrate for 15min by alcohol and deionized water respectively, drying the silicon substrate in a nitrogen atmosphere, and sputtering a zinc oxide buffer layer with the thickness of 80nm on the silicon substrate by a direct-current magnetron sputtering method (the sputtering condition is 80W in power, 150s in time, 12sccm of argon flow and 0.3 Pa);
(2) the substrate sputtered with the buffer layer is placed in a reaction kettle filled with reaction solution (70 ml; 0.02M zinc nitrate, 0.02M hexamethylenetetramine), hydrothermal reaction is carried out for 5h at 95 ℃, then the substrate is taken out, washed by deionized water and dried for 5min at 80 ℃ to obtain the zinc oxide nano rod, as shown in figure 2, the diameter of the nano rod is relatively uniform and is about 200 nm.
(3) And placing the substrate with the zinc oxide nanorods in an atomic beam deposition cavity to deposit a gallium nitride shell layer. The precursor is triethyl gallium (99.99 percent) and hydrogen-nitrogen mixed gas (the volume ratio is 1/4), the reaction temperature is 200 ℃, the plasma power is 200w, and the cycle number is 400 times. The method comprises the following specific steps: the pulse time of the triethyl gallium is 0.03s, the reaction time is 10s, the cleaning time is 40s, the plasma time of the nitrogen-hydrogen mixed gas is 10s, the cleaning is carried out for 40s again, and the steps are repeated for 400 times.
(4) And (2) dripping 500 mu l of prepared dilute sulfuric acid solution (100ml of water +3 drops of concentrated sulfuric acid, ph-1.5) on a substrate with a zinc oxide/gallium nitride core shell, reacting for 5min, heating the substrate to 60 ℃, drying the dilute sulfuric acid solution, repeating for 2 times, dripping deionized water to wash residual impurity ions on the surface, and drying at 80 ℃ to obtain the gallium nitride nanotube.
Example 4
(1) Ultrasonically cleaning the silicon substrate by alcohol and deionized water for 15min respectively, drying by nitrogen, and sputtering a zinc oxide buffer layer with the thickness of 80nm on the silicon substrate by a direct-current magnetron sputtering method (the sputtering condition is 80W, the time is 150s, the argon flow is 12sccm, and the pressure is 0.3 Pa);
(2) the substrate sputtered with the buffer layer is placed in a reaction kettle filled with reaction solution (70 ml; 0.02M zinc nitrate, 0.02M hexamethylenetetramine), hydrothermal reaction is carried out for 8h at 95 ℃, then the substrate is taken out, washing is carried out by deionized water, and drying is carried out for 5min at 80 ℃ to obtain the zinc oxide nano-rod, wherein the diameter of the nano-rod is uniform and is about 250 nm.
(3) And placing the substrate with the zinc oxide nanorods in an atomic beam deposition cavity to deposit a gallium nitride shell layer. The precursor is triethyl gallium (99.99 percent) and hydrogen-nitrogen mixed gas (the volume ratio is 1/4), the reaction temperature is 200 ℃, the plasma power is 200w, and the cycle number is 400 times. The method comprises the following specific steps: the pulse time of the triethyl gallium is 0.04s, the reaction time is 10s, the cleaning time is 40s, the plasma time of the nitrogen-hydrogen mixed gas is 10s, the cleaning is carried out for 40s again, and the steps are repeated for 400 times.
(4) And (2) dropping 300 mu l of prepared dilute sulfuric acid solution (100ml of water +3 drops of concentrated sulfuric acid, ph-1.5) on the substrate with the zinc oxide/gallium nitride core shell, reacting for 5min, heating the substrate to 60 ℃, drying the dilute sulfuric acid solution, repeating for 3 times, dropping deionized water to wash impurity ions remained on the surface, and drying at 80 ℃ to obtain the gallium nitride nanotube.
The invention is not limited to the atomic beam deposition method in the process of preparing the gallium nitride shell layer, and can also use the methods of metal organic chemical vapor deposition, pulsed laser deposition, magnetron sputtering, chemical vapor deposition and the like.
The invention provides a method for preparing a gallium nitride nanotube. The controllable preparation of the length, the inner diameter and the outer diameter of the gallium nitride nanotube can be realized. Is expected to be applied in the fields of LED, ultraviolet detector, biosensing, catalysis and the like.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.

Claims (10)

1.一种氮化镓纳米管的制备方法,其特征在于,包括如下步骤:1. a preparation method of gallium nitride nanotube, is characterized in that, comprises the steps: (1)将衬底洗净,吹干,然后采用直流磁控溅射法在衬底上溅射一层氧化锌作为缓冲层,得到有缓冲层的衬底;(1) the substrate is cleaned and dried, and then a layer of zinc oxide is sputtered on the substrate by DC magnetron sputtering as a buffer layer to obtain a substrate with a buffer layer; (2)将步骤(1)所述有缓冲层的衬底浸泡在硝酸锌与六亚甲基四胺的混合液中,然后升温进行水热反应,洗涤,烘干,得到长有氧化锌纳米棒的衬底;(2) soaking the substrate with the buffer layer described in step (1) in the mixed solution of zinc nitrate and hexamethylenetetramine, then heating up to carry out hydrothermal reaction, washing and drying to obtain nanometer zinc oxide rod substrate; (3)将步骤(2)所述长有氧化锌纳米棒的衬底放在原子束沉积腔体中沉积氮化镓壳层,得到长有氧化锌/氮化镓核壳的衬底;(3) placing the substrate with zinc oxide nanorods described in step (2) in the atomic beam deposition cavity to deposit a gallium nitride shell layer to obtain a substrate with zinc oxide/gallium nitride core shells; (4)将稀硫酸溶液滴加在长有氧化锌/氮化镓核壳的衬底上,稀硫酸溶液浸泡所述氧化锌/氮化镓核壳的衬底的表面,静置反应,加热烘干,重复2-3次后,洗涤,干燥,得到所述氮化镓纳米管。(4) drop the dilute sulfuric acid solution on the substrate with the zinc oxide/gallium nitride core-shell, soak the surface of the zinc oxide/gallium nitride core-shell substrate with the dilute sulfuric acid solution, leave it to react, and heat After drying, repeating 2-3 times, washing and drying, the gallium nitride nanotubes are obtained. 2.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(1)所述衬底为硅衬底、二氧化硅衬底、氧化铝衬底中的一种。2 . The method for preparing gallium nitride nanotubes according to claim 1 , wherein the substrate in step (1) is one of a silicon substrate, a silicon dioxide substrate, and an aluminum oxide substrate. 3 . 3.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(1)所述氧化锌的厚度为80-120nm。3 . The method for preparing gallium nitride nanotubes according to claim 1 , wherein the thickness of the zinc oxide in step (1) is 80-120 nm. 4 . 4.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,在步骤(2)所述硝酸锌与六亚甲基四胺的混合液中,硝酸锌的浓度为0.02-0.03M,六亚甲基四胺的浓度为0.02-0.03M。4. The preparation method of gallium nitride nanotubes according to claim 1, is characterized in that, in the mixed solution of zinc nitrate and hexamethylenetetramine described in step (2), the concentration of zinc nitrate is 0.02- 0.03M, the concentration of hexamethylenetetramine is 0.02-0.03M. 5.根据权利要求4所述的氮化镓纳米管的制备方法,其特征在于,在步骤(2)所述硝酸锌与六亚甲基四胺的混合液中,硝酸锌与六亚甲基四胺的摩尔比为1:1。5. the preparation method of gallium nitride nanotube according to claim 4 is characterized in that, in the mixed solution of zinc nitrate and hexamethylene tetramine described in step (2), zinc nitrate and hexamethylene tetramine The molar ratio of tetramine was 1:1. 6.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(2)所述水热反应的温度为90℃-95℃,水热反应的时间为5-8h,所述烘干的温度为60-80℃,烘干的时间为5-10min。6. The preparation method of gallium nitride nanotubes according to claim 1, wherein the temperature of the hydrothermal reaction in step (2) is 90°C-95°C, and the time of the hydrothermal reaction is 5-8h, The drying temperature is 60-80° C., and the drying time is 5-10 min. 7.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(3)中,沉积氮化镓壳层的反应温度为200-300℃,沉积氮化镓壳层的气氛为氢气和氮气的混合气氛;所述氢气与氮气的体积比为1:4。7 . The method for preparing gallium nitride nanotubes according to claim 1 , wherein in step (3), the reaction temperature for depositing the gallium nitride shell layer is 200-300° C., and the temperature for depositing the gallium nitride shell layer is 200-300° C. The atmosphere is a mixed atmosphere of hydrogen and nitrogen; the volume ratio of the hydrogen and nitrogen is 1:4. 8.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(3)中,沉积氮化镓壳层的过程包括:将三乙基镓脉冲0.03-0.04s,反应时间为10-15s,清洗时间为40-60s,氮气和氢气的混合气氛等离子体时间为10-20s,再次清洗40-60s,重复以上步骤300-400次。8. The method for preparing gallium nitride nanotubes according to claim 1, wherein in step (3), the process of depositing the gallium nitride shell layer comprises: pulse triethylgallium for 0.03-0.04s, react The time is 10-15s, the cleaning time is 40-60s, the plasma time of the mixed atmosphere of nitrogen and hydrogen is 10-20s, the cleaning time is 40-60s again, and the above steps are repeated 300-400 times. 9.根据权利要求1所述的氮化镓纳米管的制备方法,其特征在于,步骤(4)所述稀硫酸溶液的pH值为1.5-4;所述静置反应的时间为5-10min;所述加热烘干的温度为50-70℃。9 . The preparation method of gallium nitride nanotubes according to claim 1 , wherein the pH value of the dilute sulfuric acid solution in step (4) is 1.5-4; the time of the standing reaction is 5-10 min. 10 . ; The temperature of the heating and drying is 50-70°C. 10.一种由权利要求1-9任一项所述的制备方法制得的氮化镓纳米管。10. A gallium nitride nanotube prepared by the preparation method of any one of claims 1-9.
CN202010133005.7A 2020-02-29 2020-02-29 Gallium nitride nanotube and preparation method thereof Pending CN111204719A (en)

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