CN111017890A - Method for rapidly preparing MXene film with high volume specific capacitance - Google Patents

Method for rapidly preparing MXene film with high volume specific capacitance Download PDF

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CN111017890A
CN111017890A CN201911404814.0A CN201911404814A CN111017890A CN 111017890 A CN111017890 A CN 111017890A CN 201911404814 A CN201911404814 A CN 201911404814A CN 111017890 A CN111017890 A CN 111017890A
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mxene
specific capacitance
high volume
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刘宇艳
王敬枫
樊志敏
谢志民
王友善
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Harbin Institute of Technology
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Abstract

A rapid preparation method of MXene film with high volume specific capacitance belongs to the MXene material preparation field, and the specific scheme is as follows: a method for rapidly preparing MXene film with high volume specific capacitance comprises the following steps: adding an aqueous solution of an alkaline compound into the MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, then carrying out vacuum filtration on the mixed liquid A to obtain a filter cake, and drying the filter cake to obtain the MXene membrane with high volume specific capacitance. The invention overcomes the defects of low efficiency and F existing in the traditional MXene film preparation process‑The MXene film prepared by the method has excellent electrochemical performance and still maintains excellent conductivity and electromagnetic shielding performance. In addition, the preparation method has low cost and strong operability, and can be used for large-scale industrial production.

Description

Method for rapidly preparing MXene film with high volume specific capacitance
Technical Field
The invention belongs to the field of MXene material preparation, and particularly relates to a rapid preparation method of an MXene film with high volume specific capacitance.
Background
MXene is a new type of two-dimensional transition metal carbide/nitride or carbonitride, available in the general formula Mn+ 1XnTxWherein M represents a transition metal, X represents C or N, TxIt represents the MXene functional groups (-OH, ═ O and-F) which are generally obtained by selective etching of a in the MAX phase of its precursor, a representing Al, Si, etc. The dispersion liquid formed by MXene and water is electronegative due to the existence of oxygen-containing functional groups on the surface of MXene. The MXene film obtained by suction filtration has excellent conductivity, so that the MXene film has great application prospect in the fields of electrochemical energy storage, electromagnetic shielding and the like. The MXene film prepared by FaisalShahzad et al through suction filtration has conductivity of 4600S/cm, the electromagnetic interference shielding effect of MXene film with thickness of 45 μm can reach 92dB, and the electromagnetic shielding performance is the highest value of artificially synthesized material (pure MXene film) (Science 353.6304(2016): 1137-. However, the filtration process consumes time and energy, and if the concentration of the dispersion liquid is extremely low, a membrane with a certain thickness is obtained, so that the difficulty is greatly improved. In addition, MXene dispersion is easily oxidized, and the excellent performance of MXene itself is easily deteriorated even if the pumping time is too long. And the MXene film obtained by suction filtration has F-The pores are particularly underdeveloped and easily agglomerated, which greatly limits the relevant applications in the electrochemical field. Generally, graphene solves the defects by introducing some nano materials such as carbon nanotubes in the middle of the film, increases the interlayer spacing, inhibits agglomeration, and shows good performance, but the high density of the MXene film is destroyed after the materials are added, and in addition, the carbon nanotubes are double electric layer materials, so the proportion of pseudo capacitance of the MXene is reduced, and the specific capacitance is finally reduced.
Disclosure of Invention
The invention aims to overcome the defects that the traditional MXene film preparation process is time-consuming, energy-consuming and low in efficiency, and the prepared MXene film contains F-The invention provides a rapid preparation method of MXene film with high volume specific capacitance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for quickly preparing an MXene membrane with high volume specific capacitance comprises the steps of adding an aqueous solution of an alkaline compound into an MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, carrying out vacuum filtration on the mixed liquid A to obtain a filter cake, and drying the filter cake to obtain the MXene membrane with high volume specific capacitance.
Further, drying the filter cake at 20-80 ℃ for 1-10h to obtain the MXene film with high volume specific capacitance.
Further, the concentration of the MXene dispersion liquid is 0.01-20mg/mL, the concentration of the aqueous solution of the alkaline compound is 0.01-10 mol/L, and the volume ratio of the aqueous solution of the alkaline compound to the MXene dispersion liquid is 0.01-100: 1.
further, the alkaline compound includes a base and/or a strong base and a weak acid salt.
Further, the alkali comprises one or more of potassium hydroxide, barium hydroxide, ammonia water, sodium hydroxide, lithium hydroxide, calcium hydroxide and tetrabutylammonium hydroxide; the strong alkali weak acid salt comprises one or more of sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, potassium carbonate, potassium bicarbonate, potassium acetate and potassium phosphate;
further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: dispersing lithium fluoride in hydrochloric acid, and fully stirring for 1-10min at 25-60 ℃ by using a magnetic stirrer at 200-2400rpm to obtain a mixed solution B;
step 2: slowly adding the MAX phase into the mixed solution B, and magnetically stirring and reacting at the temperature of between 25 and 70 ℃ and the rpm of between 300 and 2000rpm for 0.5 to 48 hours to obtain a mixed solution C;
and step 3: and repeatedly centrifuging and cleaning the precipitate after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then diluting the obtained substrate by using water or ethanol, carrying out ultrasonic treatment for 5-60min under the power of 200-1200W, and finally centrifuging the diluted liquid at the rotating speed of 2000-5000r/min for 10-60min to obtain the supernatant, namely the MXene dispersion liquid.
Further, in the step 1, the concentration of the hydrochloric acid is 6-12M, and the mass-to-volume ratio of the lithium fluoride to the hydrochloric acid is 1-4 g: 30-60 mL.
Further, in the step 2, the mass-to-volume ratio of the MAX to the mixed solution B is 1-10g:20-80 mL.
Compared with the prior art, the invention has the beneficial effects that:
(1) the MXene membrane obtained by suction filtration by the method disclosed by the invention can be quickly prepared only by a very small amount of alkaline compounds, the method is simple, and the preparation cost is greatly reduced due to the great reduction of the suction filtration time, so that the method is very suitable for large-scale batch production.
(2) By adding soluble metal or non-metal hydroxide or strong base weak acid salt, F on MXene surface can be made-Removal of a large amount of OH with simultaneous formation of OH-(beneficial to improving specific capacitance), curling MXene nanosheets, welding a plurality of MXene nanosheets together by neutralizing negative charges carried by MXene colloids with alkali metal ions to further construct a curled MXene nano spherical aggregate with low fluorine content or even no fluorine content, and preparing the MXene dispersion liquid subjected to alkali treatment into a membrane by adopting a vacuum suction filtration self-assembly method-The finally prepared MXene film has excellent electrochemical performance, conductivity, electromagnetic shielding, low fluorine/no fluorine and certain nano-pores; overcomes the disadvantages of time and energy consumption, low efficiency and F content of the traditional MXene membrane preparation-The defects of much pores and particularly undeveloped pores and easy agglomeration; the method has great significance in the application and industrialization of the MXene film in the fields of electrochemistry, electromagnetic screens and the like.
Drawings
Fig. 1 is a schematic diagram of the MXene film production process; wherein the left figure is original MXene dispersion liquid, the middle figure is MXene dispersion liquid added with alkali, and the right figure is MXene film obtained by carrying out suction filtration on the MXene dispersion liquid added with alkali;
fig. 2 is a schematic diagram of the MXene film prepared in example 1 as a conductive path.
Detailed Description
The technical solutions of the present invention are further described below with reference to fig. 1-2 and the embodiments, but not limited thereto, and all modifications or equivalent substitutions that do not depart from the spirit and scope of the technical solutions of the present invention should be covered by the protection scope of the present invention.
Detailed description of the invention
A method for rapidly preparing MXene film with high volume specific capacitance comprises the following steps:
the method comprises the following steps: mechanically stirring 5-200mL of 0.01-20mg/mL MXene dispersion for 2-10 min;
step two: dissolving an alkaline compound in water, and mechanically stirring for 2-20min to obtain an aqueous solution of the alkaline compound, wherein the concentration of the aqueous solution of the alkaline compound is 0.01-10 mol/L;
step three: mixing the solutions prepared in the first step and the second step, wherein the volume ratio of the aqueous solution of the alkaline compound to the MXene dispersion is 0.01-100: 1, mechanically stirring for 2-20min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into an oven with the temperature of 20-80 ℃ for drying for 1-10h to obtain the MXene membrane with high volume specific capacitance.
Further, the alkaline compound comprises a base and/or a strong base weak acid salt, and the base comprises one or more of potassium hydroxide, barium hydroxide, ammonia water, sodium hydroxide, lithium hydroxide, calcium hydroxide and tetrabutylammonium hydroxide; the strong alkali weak acid salt comprises one or more of sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, potassium carbonate, potassium bicarbonate, potassium acetate and potassium phosphate.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 30-60mL of 6-12M hydrochloric acid into a plastic bottle, then dispersing 1-4g of lithium fluoride into the hydrochloric acid, and fully stirring for 1-10min at 25-60 ℃ by using a magnetic stirrer at 200-2400rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the temperature of between 25 and 70 ℃ and at the speed of between 300 and 2000rpm for 0.5 to 48 hours to obtain a mixed solution C; the volume-mass ratio of the MAX to the mixed liquid B is 1-10g:20-80 mL.
And step 3: and repeatedly centrifuging and cleaning the precipitate after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then diluting the obtained substrate by using water or ethanol, carrying out ultrasonic treatment for 5-60min under the power of 200-1200W, and finally centrifuging the diluted liquid at the rotating speed of 2000-5000r/min for 10-60min to obtain the supernatant, namely the MXene dispersion liquid.
Example 1
A method for rapidly preparing an MXene film with high volume specific capacitance specifically comprises the following steps:
the method comprises the following steps: taking 25mL of MXene dispersion liquid with the concentration of 1.2mg/mL, and mechanically stirring for 2 min;
step two: dissolving 0.55g of potassium hydroxide in 5mL of water, and mechanically stirring for 3 min;
step three: mixing the solutions prepared in the first step and the second step, and mechanically stirring for 3min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into a 50 ℃ oven for drying for 1h to obtain the MXene membrane with high volume specific capacitance.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring the mixture for 5min at room temperature by using a magnetic stirrer at the speed of 1000rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the speed of 1000rpm at 35 ℃ for 36 hours to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 200W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 1.2 mg/mL.
Example 2
A preparation method of an MXene film with high volume specific capacitance specifically comprises the following steps:
the method comprises the following steps: taking 10mL of MXene dispersion liquid with the concentration of 3mg/mL, and mechanically stirring for 3 min;
step two: dissolving 0.4g of potassium hydroxide in 20mL of water, and mechanically stirring for 4 min;
step three: mixing the solutions prepared in the first step and the second step, and mechanically stirring for 5min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into a 40 ℃ oven for drying for 1.7h to obtain the MXene membrane with high volume specific capacitance.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring for 5min at room temperature at the speed of 200rpm by using a magnetic stirrer to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the temperature of 35 ℃ at the speed of 300rpm for 36 hours to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value is neutral, then adding 100mL of water into the obtained product for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 5min under 1200W of power, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain a supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 3 mg/mL.
Example 3
A preparation method of an MXene film with high volume specific capacitance specifically comprises the following steps:
the method comprises the following steps: 40mL of MXene dispersion with the concentration of 1.5mg/mL, and mechanically stirring for 5 min;
step two: dissolving 0.25g of potassium hydroxide in 20mL of water, and mechanically stirring for 4 min;
step three: mixing the solutions obtained in the first step and the second step, and mechanically stirring for 5min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into a 50 ℃ oven for drying for 1.8h to obtain the MXene membrane with high volume specific capacitance.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring at room temperature for 5min by using a magnetic stirrer at the speed of 2400rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the temperature of 35 ℃ at the speed of 2000rpm for 36 hours to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 500W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 1.5 mg/mL.
Example 4
A preparation method of an MXene film with high volume specific capacitance specifically comprises the following steps:
the method comprises the following steps: 200mL of MXene dispersion with the concentration of 0.01mg/mL, and mechanically stirring for 10 min;
step two: 2.12g of sodium carbonate is dissolved in 2mL of water, and the solution is mechanically stirred for 20 min;
step three: mixing the solutions obtained in the first step and the second step, and mechanically stirring for 20min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into a 20 ℃ oven for drying for 10h to obtain the MXene membrane with high volume specific capacitance.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 60mL of 6M hydrochloric acid into a plastic bottle, then dispersing 4g of lithium fluoride into the hydrochloric acid, and fully stirring for 1min at 60 ℃ by using a magnetic stirrer at 2400rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the temperature of 70 ℃ at the speed of 300rpm for 48 hours to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 1g:80 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 60min under 800W of power, and finally centrifuging the diluted solution for 60min at 2000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 0.01 mg/mL.
Example 5
A preparation method of an MXene film with high volume specific capacitance specifically comprises the following steps:
the method comprises the following steps: 5mL of MXene dispersion with the concentration of 20mg/mL, and mechanically stirring for 8 min;
step two: dissolving 106g of potassium phosphate in 100mL of water, and mechanically stirring for 10 min;
step three: mixing the solutions obtained in the first step and the second step, and mechanically stirring for 10min to form a uniform mixed solution A;
step four: pouring the mixed solution A into a vacuum filtration device for filtration to obtain a filter cake, removing the filter cake, and putting the filter cake into an oven at 80 ℃ for drying for 5h to obtain the MXene membrane with high volume specific capacitance.
Further, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 30mL of 12M hydrochloric acid into a plastic bottle, then dispersing 1g of lithium fluoride into the hydrochloric acid, and fully stirring for 10min at 45 ℃ by using a magnetic stirrer at the speed of 2000rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the speed of 2000rpm for 1h at the temperature of 25 ℃ to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 10g:20 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under 1000W of power, and finally centrifuging the diluted solution for 30min at the rotating speed of 5000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 20 mg/mL.
Fig. 1 is a schematic diagram of the production process of MXene film in example 1.
Fig. 2 shows an MXene film prepared in example 1 for a conductive path to illuminate an LED lamp.
Table 1 shows the specific capacitance and conductivity of the MXene films prepared in examples 1-3, compared with pure MXene films, the pumping time of the MXene films prepared in the present invention is greatly reduced, the specific capacitance can be improved by 51% at the lowest, and in addition, the conductivity is still very high, which further illustrates the superiority of the MXene film preparation method of the present invention.
Table 1: MXene films prepared in examples 1-3 having suction filtration time, conductivity, volumetric capacitance and electromagnetic shielding effectiveness
Suction filtration time Volume specific capacitance Electrical conductivity of Electromagnetic shielding effectiveness
Pure MXene film 15060s 1320F/cm3 6563S/cm 57dB
Example 1 11s 2250F/cm3 1984S/cm 47dB
Example 2 7s 2170F/cm3 2281S/cm 48dB
Example 3 43s 1990F/cm3 2874S/cm 49dB

Claims (8)

1. A method for rapidly preparing MXene film with high volume specific capacitance is characterized by comprising the following steps: adding an aqueous solution of an alkaline compound into the MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, then carrying out vacuum filtration on the mixed liquid A to obtain a filter cake, and drying the filter cake to obtain the MXene membrane with high volume specific capacitance.
2. The method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 1, wherein: and drying the filter cake for 1-10h at the temperature of 20-80 ℃ to obtain the MXene film with high volume specific capacitance.
3. The method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 1, wherein: the concentration of the MXene dispersion liquid is 0.01-20mg/mL, the concentration of the aqueous solution of the alkaline compound is 0.01-10 mol/L, and the volume ratio of the aqueous solution of the alkaline compound to the MXene dispersion liquid is 0.01-100: 1.
4. the method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 1, wherein: the alkaline compound comprises alkali and/or strong alkali weak acid salt.
5. The method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 4, wherein: the alkali comprises one or more of potassium hydroxide, barium hydroxide, ammonia water, sodium hydroxide, lithium hydroxide, calcium hydroxide and tetrabutyl ammonium hydroxide; the strong alkali weak acid salt comprises one or more of sodium carbonate, sodium bicarbonate, sodium acetate, sodium phosphate, potassium carbonate, potassium bicarbonate, potassium acetate and potassium phosphate;
6. the method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 1, wherein: the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: dispersing lithium fluoride in hydrochloric acid, and fully stirring for 1-10min at 25-60 ℃ by using a magnetic stirrer at 200-2400rpm to obtain a mixed solution B;
step 2: slowly adding the MAX phase into the mixed solution B, and magnetically stirring and reacting at the temperature of between 25 and 70 ℃ and the rpm of between 300 and 2000rpm for 0.5 to 48 hours to obtain a mixed solution C;
and step 3: and repeatedly centrifuging and cleaning the precipitate after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then diluting the obtained substrate by using water or ethanol, carrying out ultrasonic treatment for 5-60min under the power of 200-1200W, and finally centrifuging the diluted liquid at the rotating speed of 2000-5000r/min for 10-60min to obtain the supernatant, namely the MXene dispersion liquid.
7. The method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 6, wherein: in the step 1, the concentration of the hydrochloric acid is 6-12M, and the mass volume ratio of the lithium fluoride to the hydrochloric acid is 1-4 g: 30-60 mL.
8. The method for rapidly preparing the MXene film with high volume specific capacitance as claimed in claim 6, wherein: in the step 2, the mass-to-volume ratio of the MAX to the mixed solution B is 1-10g:20-80 mL.
CN201911404814.0A 2019-12-30 2019-12-30 Method for rapidly preparing MXene film with high volume specific capacitance Pending CN111017890A (en)

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Application publication date: 20200417