CN113526507B - MXene metal nano composite material, preparation method and application - Google Patents
MXene metal nano composite material, preparation method and application Download PDFInfo
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Abstract
The invention relates to the technical field of MXene materials, in particular to a novel MXene metal nano composite material, a preparation method and application, wherein the novel MXene metal nano composite material comprises a plurality of MXene material layers; metal nanowires loaded between the MXene material layers; according to the novel MXene metal nano composite material provided by the invention, the metal nanowire intercalation is loaded between MXene material layers, the surface of the MXene material layers and the metal nanowires between the MXene material layers can be randomly combined into a metal nanowire network, so that the MXene interlayer supporting effect can be realized, the problem of interlayer collapse of the MXene material is avoided, more specific surface area of the MXene material is exposed, more active sites and interlayer energy storage space are provided, and the conductivity, electrochemical performance and stability of the MXene metal nano composite material in practical application are further improved.
Description
Technical Field
The invention relates to the technical field of MXene materials, in particular to a novel MXene metal nano composite material, a preparation method and application.
Background
MXene is a novel nano material, and has attracted close attention of researchers since the discovery in 2011. MXene materials are prepared primarily by etching MAX phase starting materials. The MXene material has high conductivity, large specific surface area, good mechanical property and certain self-reduction capability on the surface, so the MXene material has wide application in catalysis, energy storage, electromagnetic shielding, electrical devices and the like.
For example, chinese patent application (publication No. CN110841721 a) discloses an MXene two-dimensional material, a Cu/MXene catalyst, and a preparation method and an application thereof, wherein a uniformly mixed reaction system containing lithium fluoride, an acid and an MXene precursor is reacted, a mixture of a reaction product and water is vibrated by a mechanical vibration technology, and then the MXene two-dimensional material is obtained by ultrasonic treatment. It also discloses a preparation method of the Cu/MXene catalyst, which comprises the following steps: and mixing and reacting the copper source and the MXene two-dimensional material solution, centrifuging, and drying the solid obtained by centrifuging to obtain the Cu/MXene catalyst with the characteristics of high dispersibility and accurate control of the position of the active component site.
However, the existing MXene material has the problem of interlayer collapse, which causes adverse effects such as reduction of specific surface area, reduction of active sites, and absence of interlayer energy storage space of the MXene material.
Disclosure of Invention
In order to overcome the defect of interlayer collapse of the MXene material in the prior art, the novel MXene metal nanocomposite, the preparation method and the application can avoid interlayer collapse of the MXene material, improve the specific surface area, the active site and the interlayer energy storage space of the MXene material, and further improve the conductivity, the electrochemical performance and the stability of the MXene metal nanocomposite in practical application.
The invention provides a novel MXene metal nano composite material, which comprises
A plurality of MXene material layers; and the metal nanowires are loaded between the MXene material layers.
On the basis of the scheme, the MXene material comprises but is not limited to Ti 3 C 2 T x 、Ti 2 CT x 、Ti 2 NT x 、Nb 2 CT x 、Nb 4 C 3 T x 、Ta 2 CT x 、 Ta 4 C 3 T x 、V 2 CT x 、V 3 C 2 T x 、Cr 2 CT x 、Cr 3 C 2 T x 、(Ti 0 .5 Nb 0 .5 ) 2 CT x 、Ti 3 (C 0 .5 N 0 .5 ) 2 Tx or MO 2 CT x Either one or a combination of both.
On the basis of the scheme, the invention further provides a method for preparing the novel MXene metal nanocomposite, which adopts a one-pot method and comprises the following steps:
pretreating MXene raw materials;
intercalation growth of the metal nanowire;
extracting MXene metal nano composite material.
On the basis of the scheme, further, the pretreatment comprises the step of carrying out mixed ultrasonic treatment on the MXene raw material and a structure directing agent.
On the basis of the scheme, the structure directing agent is an organic solvent, and the mixing pretreatment time is 20-60min.
On the basis of the scheme, the metal nanowire intercalation growth further comprises the steps of adding a metal precursor and a reducing agent into the pretreated mixture, heating and stirring under a protective atmosphere to decompose the metal precursor, adsorbing and inserting positively charged metal ions into the MXene material layers, and growing the metal nanowire under the action of the structure directing agent.
On the basis of the scheme, further, the ratio of the metal precursor to the reducing agent is 1:1-2 by weight; the metal precursor is a metal inorganic salt, which includes, but is not limited to, metal chlorides, metal nitrates, metal sulfates, and metal sulfites.
On the basis of the scheme, further, the protective atmosphere includes but is not limited to one or a combination of any of argon, nitrogen and helium.
On the basis of the scheme, further, the step of extracting the MXene metal nanocomposite comprises the steps of cooling the mixture after the intercalation growth of the metal nanowires is completed to room temperature, sequentially carrying out ultrasonic treatment, centrifugal purification and precipitate extraction, and extracting to obtain the MXene metal nanocomposite.
On the basis of the scheme, the invention further provides an application of the MXene metal nanocomposite in electrical devices and thin films, wherein the MXene metal nanocomposite is the novel MXene metal nanocomposite or the composite prepared by the preparation method of the novel MXene metal nanocomposite.
Compared with the prior art, the novel MXene metal nano composite material, the preparation method and the application have the advantages that the metal nanowire intercalation is loaded between the MXene material layers, the metal nanowires positioned on the surfaces of the MXene material layers and between the MXene material layers can be randomly combined into the metal nanowire network, the MXene interlayer supporting effect can be achieved, the problem of interlayer collapse of the MXene material is avoided, the MXene material is exposed to more specific surface areas, more active sites and interlayer energy storage spaces are provided, and the conductivity, the electrochemical performance and the stability of the MXene metal nano composite material in practical application are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a novel MXene metal nanocomposite provided by the present invention;
fig. 2 is a transmission electron microscope image of the novel MXene metal nanocomposite provided by the invention;
fig. 3 is a flow chart of the preparation of the novel MXene metal nanocomposite provided by the invention;
fig. 4 is a schematic view of the growth of a metal nanowire of the novel MXene metal nanocomposite provided by the present invention;
fig. 5 is an EDS spectrum of the novel MXene metal nanocomposite provided by the present invention;
FIG. 6 is a Tyndall effect diagram of a dispersion provided by the present invention;
fig. 7 is an IV characteristic diagram of the MXene metal nanocomposite provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Furthermore, the technical features designed in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1 and fig. 2, the novel MXene metal nanocomposite provided by the invention comprises a plurality of layers of MXene material; and the metal nanowires are loaded between the MXene material layers.
In specific implementation, as shown in fig. 1 and fig. 2, the metal nanowire intercalation layer grows and is loaded between the MXene material layers, the metal nanowires are loaded on the surfaces and the layers of the MXene material layers, and the metal nanowires positioned on the surfaces and the layers of the MXene material layers can be randomly combined into a metal nanowire network, so that a good supporting effect between the MXene layers can be achieved, the problem of interlayer collapse of the MXene material is solved, the MXene material is exposed to more specific surface areas, more active sites and more interlayer energy storage spaces are provided, and the conductivity, the electrochemical performance and the stability of the MXene metal nanocomposite in practical application are improved.
In this embodiment, MXene materials include but are not limited to Ti 3 C 2 T x 、Ti 2 CT x 、Ti 2 NT x 、Nb 2 CT x 、Nb 4 C 3 T x 、Ta 2 CT x 、 Ta 4 C 3 T x 、V 2 CT x 、V 3 C 2 T x 、Cr 2 CT x 、Cr 3 C 2 T x 、(Ti 0 .5 Nb 0 .5 ) 2 CT x 、Ti 3 (C 0 .5 N 0 .5 ) 2 Tx or MO 2 CT x In any one or two combinations, the MXene material can also be prepared by selecting a proper MAX phase raw material according to actual needs through the prior art or documents, and details are not repeated here.
As shown in fig. 3 and 4, the method for preparing the novel MXene metal nanocomposite adopts a one-pot method according to the following steps:
step 1, MXene raw materials are pretreated;
and 3, extracting the MXene metal nano composite material.
In specific implementation, MXene raw material is taken in a three-neck flask, a structure-directing agent is added, the whole flask is placed in cold water for mixed ultrasonic pretreatment, wherein the ratio of the MXene raw material to the structure-directing agent can be 0.1-1g:5-20ml, the structure directing agent can be an organic solvent, and the time of mixed ultrasonic pretreatment can be 20-60min;
adding a metal precursor and a reducing agent into the mixture pretreated in the step 1, wherein the ratio of the metal precursor to the reducing agent is 1:1-2 by weight; the metal precursor may be a metal inorganic salt including, but not limited to, metal chlorides, metal nitrates, metal sulfates, and metal sulfites;
then, placing the three-neck flask on a magnetic stirring table, continuously introducing a protective atmosphere and adding magnetons, wherein the protective atmosphere comprises but is not limited to one or a combination of any of argon, nitrogen and helium, and preferably, the purity of the protective atmosphere is more than 90%; heating and stirring the mixture under the protective atmosphere to enable the metal precursor in the three-neck flask to react with the MXene material;
as shown in fig. 4, the metal precursor is decomposed in a liquid phase system, and as the surface of the MXene material is negatively charged after etching, the positively charged metal ions are electrostatically adsorbed, and under continuous stirring, the positively charged metal ions are adsorbed and inserted between the MXene layers, and the metal nanowires are grown under the action of the structure directing agent.
After the intercalation growth reaction of the metal nanowires is finished, cooling the mixture subjected to intercalation growth of the metal nanowires to room temperature, then leading the mixture out of a three-neck flask, sequentially carrying out ultrasonic treatment, centrifugal purification and precipitate taking, wherein the ultrasonic treatment and the centrifugal treatment can be circulated for 2-5 times, and the ultrasonic treatment or the centrifugal treatment can be carried out for 2-5min each time; ultrasonic purification, centrifugal purification and sediment extraction belong to common technical means in the prior art, and are not described in detail herein.
As shown in fig. 5, by the element analysis of the energy spectrum, the existence of titanium, oxygen, carbon, fluorine and copper elements in the MXene metal nanocomposite provided by the present invention can be further proved, which indicates that the MXene metal nanocomposite is successfully prepared.
The metal nanowires are intercalated and grown and loaded between the MXene material layers, the metal nanowires positioned on the surfaces of the MXene material layers and between the MXene material layers can be randomly combined into a metal nanowire network, so that a good supporting effect between the MXene layers can be achieved, the problem of interlayer collapse of the MXene material is avoided, the MXene material is exposed to more specific surface areas, more active sites and interlayer energy storage spaces are provided, and the conductivity, the electrochemical performance and the stability of the MXene metal nano composite material in practical application are further improved.
Example 1
Taking 0.1g of MXene raw material, placing the MXene raw material in a three-neck flask, adding 5ml of structure directing agent, and placing the whole flask in cold water for mixed ultrasonic pretreatment; in this example, MXene as a raw material was Ti 3 C 2 T x The structure directing agent adopts oleylamine, the ultrasonic treatment time is 20min, and the oleylamine is fully soaked in Ti 3 C 2 T x ；
Then, adding a metal precursor and a reducing agent into the pretreated mixture, in the embodiment, adding 0.1g of copper chloride serving as the metal precursor and 0.1g of nickel acetylacetonate serving as the reducing agent, then placing the three-neck flask on a magnetic stirring table, continuously introducing nitrogen and adding magnetons, then heating to 180 ℃, stirring and reacting for 4 hours to enable the mixture in the three-neck flask to react, namely, the copper chloride and the Ti 3 C 2 T x Reacting, adsorbing and inserting positively charged metal ions into MXene layers, and growing metal nanowires under the action of oleylamine;
and finally, after the mixture is cooled to room temperature, leading the mixture out of the three-neck flask, sequentially carrying out ultrasonic purification and centrifugal purification by using normal hexane, taking out the precipitate, wherein ultrasonic purification and centrifugal purification are respectively carried out for 2 times, and the ultrasonic purification or centrifugal purification time is respectively 2min each time, and extracting to obtain the novel MXene metal nanocomposite.
Example 2
Taking 0.1g of MXene raw material, placing the MXene raw material in a three-neck flask, adding 10ml of structure directing agent, and placing the whole flask in cold water for mixed ultrasonic pretreatment; in this example, MXene was Ti as a raw material 2 CT x The structure guiding agent adopts oleylamine, the ultrasonic treatment time is 30min, so that the oleylamine can fully soak Ti 2 CT x ；
Then, adding a metal precursor and a reducing agent into the pretreated mixture, in the embodiment, adding 0.1g of copper chloride as the metal precursor and 0.15g of nickel acetylacetonate as the reducing agent, then placing the three-neck flask on a magnetic stirring table, continuously introducing helium gas into the three-neck flask and adding magnetons, subsequently heating to 180 ℃, stirring and reacting for 4 hours to enable the mixture in the three-neck flask to react, namely, the copper chloride and the Ti 2 CT x Reacting, adsorbing and inserting positively charged metal ions into MXene layers, and growing metal nanowires under the action of oleylamine;
and finally, after the mixture is cooled to room temperature, leading the mixture out of the three-neck flask, sequentially carrying out ultrasonic purification and centrifugal purification by using normal hexane, taking out the precipitate, wherein ultrasonic purification and centrifugal purification are respectively carried out for 3 times, and the ultrasonic purification or centrifugal purification is respectively carried out for 3min each time, and extracting to obtain the novel MXene metal nanocomposite.
Example 3
Taking 0.1g of MXene raw material, placing the MXene raw material in a three-neck flask, adding 20ml of structure directing agent, and placing the whole flask in cold water for mixed ultrasonic pretreatment; in this example, MXene was Ti as a raw material 2 NT x The structure guiding agent adopts oleylamine, the ultrasonic treatment time is 40min, so that the oleylamine can fully soak Ti 2 NT x ；
Then, adding a metal precursor and a reducing agent into the pretreated mixture, in the embodiment, adding 0.1g of copper chloride as the metal precursor and 0.2g of nickel acetylacetonate as the reducing agent, then placing the three-neck flask on a magnetic stirring table, continuously introducing argon gas into the three-neck flask and adding magnetons, subsequently heating to 180 ℃, stirring and reacting for 4 hours to enable the mixture in the three-neck flask to react, namely, the copper chloride and the Ti 2 NT x Reacting, adsorbing and inserting positively charged metal ions into MXene layers, and growing metal nanowires under the action of oleylamine;
and finally, after the mixture is cooled to room temperature, leading the mixture out of the three-neck flask, sequentially carrying out ultrasonic purification and centrifugal purification by using normal hexane, taking out the precipitate, wherein the ultrasonic purification and the centrifugal purification are respectively carried out for 4 times, and the ultrasonic purification or the centrifugal purification is respectively carried out for 4min each time, and extracting to obtain the novel MXene metal nano composite material.
Using Nb 2 CT x 、Nb 4 C 3 T x 、Ta 2 CT x 、 Ta 4 C 3 T x 、V 2 CT x 、V 3 C 2 T x 、Cr 2 CT x 、Cr 3 C 2 T x 、(Ti 0 .5 Nb 0 .5 ) 2 CT x 、Ti 3 (C 0 .5 N 0 .5 ) 2 Tx or MO 2 CT x The preparation method and the steps for preparing the novel MXene metal nanocomposite from the MXene material have the same principle as the above embodiment, and are not repeated herein.
As shown in table 1, comparative examples 1 and 2 are the prior art in which metal salt particles are mixed with hydrofluoric acid to prepare a solution, and then MAX powder is put into the solution and stirred; and after the reaction is finished, centrifuging the reaction solution, washing and vacuum-drying the solid product obtained after centrifugation to obtain the MXene-metal composite material, wherein the MXene-metal composite material consists of an MXene material and metal particles coated on the surface of the MXene material.
As shown in tables 1 and 2, the novel MXene metal nanocomposite prepared by the preparation method of the novel MXene metal nanocomposite provided by the invention avoids the problem of interlayer collapse of the MXene material, and further, the specific surface area and the volume capacitance are superior to those of the comparative example 1 and the comparative example 2, so that the MXene material is exposed to more specific surface area, and more active sites and interlayer energy storage spaces are provided, thereby ensuring the electrochemical performance and the stability of the MXene metal nanocomposite.
TABLE 1
TABLE 2
The invention also provides the application of the novel MXene metal nanocomposite material and the preparation method of the novel MXene metal nanocomposite material in electrical devices and films.
In specific implementation, the extracted novel MXene metal nano composite material is transferred onto a substrate by a transfer method, or can be made into a self-supporting film, and the MXene metal nano composite material device with the metal nanowire intercalation, which can be applied to the novel MXene metal nano composite material, can be finally obtained by post-treatment operation, such as application of a gas sensor and the like.
In this embodiment, the extracted novel MXene metal nanocomposite can be stored in a dispersion and then transferred to a substrate by a transfer method for subsequent use; the dispersion liquid comprises at least one of deionized water, methanol, ethanol, isopropanol or n-hexane;
as shown in fig. 6 and 7, the MXene-copper nanowire composite material has good dispersibility in isopropanol through a dispersion solution tyndall effect diagram; according to the IV characteristic diagram of the MXene metal nanowire composite material, the MXene metal nanowire composite material provided by the invention has excellent electrical characteristics.
Compared with the prior art, the novel MXene metal nano composite material, the preparation method and the application have the advantages that the metal nanowire intercalation is loaded between the MXene material layers, the metal nanowires positioned on the surfaces of the MXene material layers and between the MXene material layers can be randomly combined into the metal nanowire network, the MXene interlayer supporting effect can be achieved, the problem of interlayer collapse of the MXene material is avoided, the MXene material is exposed to more specific surface areas, more active sites and interlayer energy storage spaces are provided, and the conductivity, the electrochemical performance and the stability of the MXene metal nano composite material in practical application are improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. The preparation method of the MXene metal nanocomposite is characterized in that the MXene metal nanocomposite comprises a plurality of MXene material layers and metal nanowires loaded between the MXene material layers, and the preparation method is characterized by adopting a one-pot method and comprises the following steps:
pretreating MXene raw materials;
the pretreatment comprises the step of carrying out mixed ultrasonic treatment on the MXene raw material and a structure directing agent; the structure directing agent is oleylamine;
adding a metal precursor and a reducing agent into the pretreated mixture, heating and stirring the mixture under a protective atmosphere to decompose the metal precursor, adsorbing and inserting positively charged metal ions into the MXene material layers, and growing the metal nanowire under the action of the structure directing agent, wherein the ratio of the metal precursor to the reducing agent is 1:1-2 by weight, and the reducing agent is nickel acetylacetonate; the metal precursor is metal inorganic salt copper chloride;
extracting MXene metal nano composite material.
2. The method of preparing MXene metal nanocomposite of claim 1, wherein: the pretreatment time is 20-60min.
3. The method of preparing MXene metal nanocomposite of claim 1, wherein: the protective atmosphere is one or the combination of any more of argon, nitrogen and helium.
4. The method of preparing MXene metal nanocomposite of claim 1, wherein: the MXene metal nano composite material extraction method comprises the steps of cooling a mixture which completes intercalation growth of the metal nanowires to room temperature, sequentially carrying out ultrasonic treatment, centrifugal purification and precipitate extraction, and extracting to obtain the MXene metal nano composite material.
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