CN112076772A - Metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and preparation method thereof - Google Patents

Metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and preparation method thereof Download PDF

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CN112076772A
CN112076772A CN202010902585.1A CN202010902585A CN112076772A CN 112076772 A CN112076772 A CN 112076772A CN 202010902585 A CN202010902585 A CN 202010902585A CN 112076772 A CN112076772 A CN 112076772A
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quantum dot
nanotube array
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王玮
康琪
刘天宇
汪敏
柏寄荣
邓瑶瑶
许�鹏
孙潇楠
张金涛
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Changzhou Institute of Technology
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Abstract

The invention belongs to the technical field of nano material preparation, and particularly relates to a metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and a preparation method thereof. The preparation method comprises the following steps: (1) large-size semiconductor type MoS by adopting manual grinding method2Grinding the block to obtain semiconductor type MoS2Powder; (2) to semiconductor type MoS2Performing lithium intercalation treatment on the powder; (3) intercalation treated semiconductor type MoS of lithium2Dispersing the powder in a solvent, performing ultrasonic treatment, and performing centrifugal separation to obtain the metal MoS2A quantum dot solution; (4) putting TiN nanotube array in metal MoS2In a quantum dot solution, thenUltrasonic treatment, soaking and drying are carried out again to obtain the metal MoS2A TiN nanotube array composite material modified by quantum dots. Metal MoS of the invention2The TiN nanotube array composite material modified by the quantum dots has excellent electro-catalytic performance and stability.

Description

Metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and a preparation method thereof.
Background
MoS2Has excellent physical and chemical properties and has important application prospect in the fields of electro-catalysis, biosensing and the like. MoS2The size and shape regulation and the corresponding physical and chemical properties of the composite material become research hotspots in material science and related fields in recent years. Just MoS2As quantum dots have the characteristics of small size, large specific surface area, more exposed edge active sites and the like, the quantum dots show excellent electrocatalytic performance and can be applied to electrocatalytic hydrogen evolution reaction and high-sensitivity sensors. However, thermodynamically stable MoS2Is of a semiconductor type, and a semiconductor type MoS2Because of its weak electron transport ability, its electrocatalytic performance needs to be further improved, and the metal type MoS2Has good electron transmission capability, so that the metal type MoS2The quantum dots have wider application prospect in the field of electrocatalysis. On the other hand, MoS2The quantum dots are easy to agglomerate in a disperse phase medium to reduce the electrocatalytic performance of the quantum dots, so that the application of the quantum dots is limited. The titanium nitride nano material is a material with good physical and chemical propertiesShowing thermodynamic stability, good conductivity, good biocompatibility and the like.
Disclosure of Invention
In order to solve the problem of MoS in the prior art2The invention aims to provide a metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and a preparation method thereof, wherein the preparation method has the advantages of simple process and convenience for industrial production.
The invention is realized by the following technical scheme:
metal type MoS2The preparation method of the quantum dot modified TiN nanotube array composite material specifically comprises the following steps:
(1) in a semiconductor type MoS2Grinding the block by a manual grinding method to obtain the semiconductor MoS2Powder;
(2) in a glove box in an anhydrous and oxygen-free environment, inert gas is used as protective gas, and butyl lithium solution is adopted to react the semiconductor type MoS2Performing lithium intercalation treatment on the powder;
(3) intercalation treated semiconductor type MoS of lithium2The powder was dispersed in a solvent and subsequently sonicated to obtain a stripped MoS2-solvent mixture, followed by centrifugation to obtain the MoS of metal type2A quantum dot solution;
(4) putting the TiN nanotube array in the metal type MoS in the step (3)2Sequentially carrying out ultrasonic treatment, soaking and drying in the quantum dot solution to obtain the metal MoS2A TiN nanotube array composite material modified by quantum dots.
Preferably, the manual grinding method in the step (1) is specifically as follows: the semiconductor type MoS2Putting the block into ethanol or isopropanol to obtain a mixed solution, then putting the mixed solution into an agate mortar, manually grinding for 60min, and naturally drying after the ethanol or isopropanol is evaporated to obtain the semiconductor MoS2And (3) powder.
Preferably, the semiconductor-type MoS2The size of the block is 6 μm, halfConductor type MoS2The size of the powder is < 1 μm;
the ethanol or the isopropanol is added in an amount of the semiconductor type MoS2The mass concentration of the block in the mixed liquid is 100 mg/mL.
Preferably, the water content and the oxygen content in the glove box of the anhydrous oxygen-free environment in the step (2) are both less than 1ppm, the inert gas is one or more of nitrogen, argon and helium, and the purity of the inert gas is 99.99%.
Preferably, the butyl lithium solution in the step (2) is a n-hexane solution of butyl lithium, the molar concentration of the butyl lithium in the butyl lithium solution is 2.5mol/L, the amount of the butyl lithium solution is calculated by the volume of the butyl lithium, and the butyl lithium and the semiconductor type MoS are calculated by the volume of the butyl lithium2The volume mass ratio of the powder is 500 mu L to 20 mg.
Preferably, the solvent in the step (3) is deionized water or ethanol, and the semiconductor type MoS2The mass-volume ratio of the powder to the solvent is (10-30) mg:20mL, and the ultrasonic treatment time is 30 min.
Preferably, the number of times of the centrifugation in the step (3) is 3, and the operation is that: firstly, centrifuging for 10min at the rotating speed of 600rpm, and taking primary supernatant; then, carrying out centrifugal separation on the primary supernatant at the rotation speed of 10000rpm, and taking a secondary supernatant; finally, the secondary supernatant is further purified and centrifugally separated at the rotating speed of 15000rpm, and the obtained supernatant is metal MoS2A quantum dot solution.
Preferably, the metal type MoS2The size of the quantum dots is 3-10 nm.
Preferably, the metal type MoS in the step (4)2Metal type MoS in quantum dot solution2The mass concentration of the quantum dots is 0.5-1.5mg/mL, the ultrasonic treatment time is 10s, the soaking time is 2min, and the drying is drying in an oven at the temperature of 60 ℃ for 60 min.
The invention also aims to provide the metal type MoS prepared by the method2The quantum dot modified TiN nanotube array composite material, specifically, TiN nanotubes vertically grown on Ti sheetOn a substrate, the metal type MoS2The quantum dots are loaded on the outer surface and the inner surface of the TiN nano-tube, the outer diameter of the TiN nano-tube is 60-90nm, and the inner diameter of the TiN nano-tube is 20-30 nm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention firstly carries out lithium intercalation treatment to make the semiconductor type MoS2Powder processing into metal mold MoS2The quantum dots are subjected to ultrasonic treatment, soaking and drying to obtain the metal MoS2The TiN nanotube array composite material modified by the quantum dots has simple and feasible preparation process and wide practical application value and industrial production prospect.
(2) The invention relates to a semiconductor type MoS2Processing into metal MoS2The quantum dots improve the electron transmission capability of the catalyst, so that the electrocatalysis performance is improved; on the other hand, the metal type MoS2The quantum dots are compounded on the outer surface and the inner surface of the TiN nanotube array to obtain the nano composite material with stable structure and excellent performance, and the nano composite material has metal MoS2The electrocatalytic performance of the quantum dots and the thermodynamic stability and good conductive performance of the titanium nitride nanotube array solve the problem of single MoS2The easy agglomeration of quantum dots leads to the metal type MoS2The TiN nanotube array composite material modified by the quantum dots is expected to be applied to an enzyme-free hydrogen peroxide electrochemical sensor.
Drawings
FIG. 1 shows a MoS of the invention2The structure schematic diagram of the quantum dot modified TiN nanotube array composite material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
Metal type MoS2The preparation method of the quantum dot modified TiN nanotube array composite material specifically comprises the following steps:
(1) in a semiconductor type MoS2Grinding the block by hand grinding method to obtain semiconductor MoS with size of 6 μm2Putting the block into ethanol or isopropanol to obtain a mixed solution with the mass concentration of 100mg/mL, then putting the mixed solution into an agate mortar, manually grinding for 60min, evaporating the ethanol or isopropanol, and naturally drying to obtain the semiconductor type MoS with the size of less than 1 mu m2Powder;
(2) in a glove box in an anhydrous and oxygen-free environment with water content and oxygen content less than 1ppm, inert gas (nitrogen with the purity of 99.99%) is taken as protective gas, and butyl lithium solution with the butyl lithium molar concentration of 2.5mol/L is adopted to carry out reaction on the semiconductor MoS2Soaking the powder in a room temperature environment for lithium intercalation treatment, wherein the butyl lithium and the semiconductor MoS are2The volume mass ratio of the powder is 500 mu L to 20 mg;
(3) intercalation treated semiconductor type MoS of lithium220mg of the powder was dispersed in 20mL of deionized water and subsequently sonicated for 30min to yield stripped MoS2Solvent mixture, then on stripped MoS2-centrifuging the solvent mixture: firstly, centrifuging for 10min at the rotating speed of 600rpm, and taking primary supernatant; then the primary supernatant is centrifugally separated at 10000rpm, and a second supernatant is takenSecondary supernatant fluid; finally, the secondary supernatant is further purified and centrifugally separated at the rotating speed of 15000rpm, and the obtained supernatant is metal MoS with the mass concentration of 1mg/mL2Quantum dot solution of said metal type MoS2The size of the quantum dots is 3-10 nm;
(4) putting the TiN nanotube array material into the metal type MoS in the step (3)2Sequentially carrying out ultrasonic treatment for 10s, soaking for 2min and drying in an oven at 60 ℃ for 60min in a quantum dot solution at room temperature environment to obtain metal MoS2A TiN nanotube array composite material modified by quantum dots.
As shown in FIG. 1, the metal type MoS prepared in this example2The TiN nanotube array composite material modified by quantum dots is characterized in that TiN nanotubes vertically grow on a Ti sheet substrate, and the metal MoS2The quantum dots are loaded on the outer surface and the inner surface of the TiN nano-tube, the outer diameter of the TiN nano-tube is 60-90nm, and the inner diameter of the TiN nano-tube is 20-30 nm.
Example 2
Metal type MoS2The preparation method of the quantum dot modified TiN nanotube array composite material specifically comprises the following steps:
(1) in a semiconductor type MoS2Grinding the block by hand grinding method to obtain semiconductor MoS with size of 6 μm2Putting the block into ethanol or isopropanol to obtain a mixed solution with the mass concentration of 100mg/mL, then putting the mixed solution into an agate mortar, manually grinding for 60min, evaporating the ethanol or isopropanol, and naturally drying to obtain the semiconductor type MoS with the size of less than 1 mu m2Powder;
(2) in a glove box in an anhydrous and oxygen-free environment with water content and oxygen content less than 1ppm, inert gas (argon with the purity of 99.99%) is taken as protective gas, and butyl lithium solution with the butyl lithium molar concentration of 2.5mol/L is adopted to treat the semiconductor MoS2Soaking the powder in a room temperature environment for lithium intercalation treatment, wherein the butyl lithium and the semiconductor MoS are2The volume mass ratio of the powder is 500 mu L to 20 mg;
(3) intercalation treated semiconductor type MoS of lithium2Powder 10mg pointDispersing in 20mL deionized water, and then carrying out ultrasonic treatment for 30min to obtain the stripped MoS2Solvent mixture, then on stripped MoS2-centrifuging the solvent mixture: firstly, centrifuging for 10min at the rotating speed of 600rpm, and taking primary supernatant; then, carrying out centrifugal separation on the primary supernatant at the rotation speed of 10000rpm, and taking a secondary supernatant; finally, the secondary supernatant is further purified and centrifugally separated at the rotating speed of 15000rpm, and the obtained supernatant is metal MoS with the mass concentration of 0.5mg/mL2Quantum dot solution of said metal type MoS2The size of the quantum dots is 3-10 nm;
(4) putting the TiN nanotube array material into the metal type MoS in the step (3)2Sequentially carrying out ultrasonic treatment for 10s, soaking for 2min and drying in an oven at 60 ℃ for 60min in a quantum dot solution at room temperature environment to obtain metal MoS2A TiN nanotube array composite material modified by quantum dots.
As shown in FIG. 1, the metal type MoS prepared in this example2The TiN nanotube array composite material modified by quantum dots is characterized in that TiN nanotubes vertically grow on a Ti sheet substrate, and the metal MoS2The quantum dots are loaded on the outer surface and the inner surface of the TiN nano-tube, the outer diameter of the TiN nano-tube is 60-90nm, and the inner diameter of the TiN nano-tube is 20-30 nm.
Example 3
Metal type MoS2The preparation method of the quantum dot modified TiN nanotube array composite material specifically comprises the following steps:
(1) in a semiconductor type MoS2Grinding the block by hand grinding method to obtain semiconductor MoS with size of 6 μm2Putting the block into ethanol or isopropanol to obtain a mixed solution with the mass concentration of 100mg/mL, then putting the mixed solution into an agate mortar, manually grinding for 60min, evaporating the ethanol or isopropanol, and naturally drying to obtain the semiconductor type MoS with the size of less than 1 mu m2Powder;
(2) in a glove box with water content and oxygen content less than 1ppm in an anhydrous and oxygen-free environment, inert gas (nitrogen with purity of 99.99%) is used as protective gasThe semiconductor MoS is treated by butyl lithium solution with butyl lithium molar concentration of 2.5mol/L2Soaking the powder in a room temperature environment for lithium intercalation treatment, wherein the butyl lithium and the semiconductor MoS are2The volume mass ratio of the powder is 500 mu L to 20 mg;
(3) intercalation treated semiconductor type MoS of lithium2The powder 30mg was dispersed in 20mL deionized water and subsequently sonicated for 30min to yield stripped MoS2Solvent mixture, then on stripped MoS2-centrifuging the solvent mixture: firstly, centrifuging for 10min at the rotating speed of 600rpm, and taking primary supernatant; then, carrying out centrifugal separation on the primary supernatant at the rotation speed of 10000rpm, and taking a secondary supernatant; finally, the secondary supernatant is further purified and centrifugally separated at the rotating speed of 15000rpm, and the obtained supernatant is metal MoS with the mass concentration of 1.5mg/mL2Quantum dot solution of said metal type MoS2The size of the quantum dots is 3-10 nm;
(4) putting the TiN nanotube array material into the metal type MoS in the step (3)2Sequentially carrying out ultrasonic treatment for 10s, soaking for 2min and drying in an oven at 60 ℃ for 60min in a quantum dot solution at room temperature environment to obtain metal MoS2A TiN nanotube array composite material modified by quantum dots.
As shown in FIG. 1, the metal type MoS prepared in this example2The TiN nanotube array composite material modified by quantum dots is characterized in that TiN nanotubes vertically grow on a Ti sheet substrate, and the metal MoS2The quantum dots are loaded on the outer surface and the inner surface of the TiN nano-tube, the outer diameter of the TiN nano-tube is 60-90nm, and the inner diameter of the TiN nano-tube is 20-30 nm.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (10)

1. Metal type MoS2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized by comprising the following steps:
(1) in a semiconductor type MoS2Grinding the block by a manual grinding method to obtain the semiconductor MoS2Powder;
(2) in a glove box in an anhydrous and oxygen-free environment, inert gas is used as protective gas, and butyl lithium solution is adopted to react the semiconductor type MoS2Performing lithium intercalation treatment on the powder;
(3) intercalation treated semiconductor type MoS of lithium2The powder was dispersed in a solvent and subsequently sonicated to obtain a stripped MoS2-solvent mixture, followed by centrifugation to obtain the MoS of metal type2A quantum dot solution;
(4) putting the TiN nanotube array in the metal type MoS in the step (3)2Sequentially carrying out ultrasonic treatment, soaking and drying in the quantum dot solution to obtain the metal MoS2A TiN nanotube array composite material modified by quantum dots.
2. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the manual grinding method in the step (1) specifically comprises the following steps: the semiconductor type MoS2Putting the block into ethanol or isopropanol to obtain a mixed solution, then putting the mixed solution into an agate mortar, manually grinding for 60min, and naturally drying after the ethanol or isopropanol is evaporated to obtain the semiconductor MoS2And (3) powder.
3. The MoS of claim 2, of a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the semiconductor MoS2The size of the block is 6 μm, and the semiconductor type MoS2The size of the powder is < 1 μm;
the ethanol or the isopropanol is added in an amount of the semiconductor type MoS2The mass concentration of the block in the mixed liquid is 100 mg/mL.
4. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that in the step (2), the water content and the oxygen content in the glove box in the anhydrous oxygen-free environment are both less than 1ppm, the inert gas is one or more of nitrogen, argon and helium, and the purity of the inert gas is 99.99%.
5. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that in the step (2), the butyl lithium solution is a butyl lithium n-hexane solution, the molar concentration of butyl lithium in the butyl lithium solution is 2.5mol/L, the using amount of the butyl lithium solution is calculated by the volume of butyl lithium, and the butyl lithium and semiconductor MoS are calculated by the volume of the butyl lithium2The volume mass ratio of the powder is 500 mu L to 20 mg.
6. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the solvent in the step (3) is deionized water or ethanol, and the semiconductor MoS2The mass-volume ratio of the powder to the solvent is (10-30) mg:20mL, and the ultrasonic treatment time is 30 min.
7. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the centrifugal separation frequency in the step (3) is 3, and the preparation method specifically comprises the following steps: firstly, centrifuging for 10min at the rotating speed of 600rpm, and taking primary supernatant; then, carrying out centrifugal separation on the primary supernatant at the rotation speed of 10000rpm, and taking a secondary supernatant; finally, the secondary supernatant is further purified and centrifugally separated at the rotating speed of 15000rpm, and the obtained supernatant is metal MoS2A quantum dot solution.
8. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the metal MoS2The size of the quantum dots is 3-10 nm.
9. The MoS of claim 1, which is a metal type2The preparation method of the quantum dot modified TiN nanotube array composite material is characterized in that the metal MoS in the step (4)2Metal type MoS in quantum dot solution2The mass concentration of the quantum dots is 0.5-1.5mg/mL, the ultrasonic treatment time is 10s, the soaking time is 2min, and the drying is drying in an oven at the temperature of 60 ℃ for 60 min.
10. MoS of the metal type prepared by the process according to any one of claims 1 to 92The quantum dot modified TiN nanotube array composite material is characterized in that TiN nanotubes vertically grow on a Ti sheet substrate, and the metal MoS2The quantum dots are loaded on the outer surface and the inner surface of the TiN nano-tube, the outer diameter of the TiN nano-tube is 60-90nm, and the inner diameter of the TiN nano-tube is 20-30 nm.
CN202010902585.1A 2020-09-01 2020-09-01 Metal type molybdenum disulfide quantum dot modified TiN nanotube array composite material and preparation method thereof Pending CN112076772A (en)

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