CN112935274B - Method for growing high-entropy alloy nanoparticles on flexible substrate - Google Patents
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C—CHEMISTRY; METALLURGY
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
- C23C18/145—Radiation by charged particles, e.g. electron beams or ion irradiation
Abstract
The invention provides a method for growing high-entropy alloy nanoparticles on a flexible substrate, which comprises the following steps: obtaining a flexible substrate; growing a three-dimensional graphene film with a preset shape on the flexible substrate by adopting a laser direct writing technology; obtaining a precursor solution of the high-entropy alloy nanoparticles; dropwise adding the precursor solution to the three-dimensional graphene film to form a pretreated sample; and carrying out radiation heating treatment on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology to obtain the high-entropy alloy nanoparticles. Based on the technical scheme, the size uniformity of the high-entropy alloy nanoparticles and the total loading capacity of the alloy can be effectively improved; and effectively avoid causing high-temperature thermal damage to the flexible substrate; meanwhile, the pulse laser pyrolysis growth mechanism is also beneficial to obtaining the high-entropy alloy nanoparticles with single phase.
Description
Technical Field
The invention relates to the technical field of nano synthesis, in particular to a method for growing high-entropy alloy nanoparticles on a flexible substrate.
Background
The flexible electronics is a new electronic technology for manufacturing organic/inorganic functional materials, electronic devices or systems on the flexible substrate, has the characteristics of lightness, thinness, portability, wearability and the like, can realize the high-efficiency fusion of information with people, objects and environments, and has wide application prospects in the fields of information, energy, medical treatment, national defense and the like. The high-entropy alloy nanoparticles are novel nanomaterials which are composed of 5 or more metal elements and have single phases, and have attracted much attention in the fields of catalysis, energy, sensing and the like in recent years.
Although the traditional wet chemical method is often used for synthesizing alloy nanoparticles with different shapes, sizes and structures, the preparation of multi-element alloy nano materials with more than 3 element combinations is difficult. Some schemes in the prior art can synthesize five-membered high-entropy alloy nanoparticles by adopting a solvothermal method, but the method has no universality and is particularly not suitable for synthesizing the high-entropy alloy nanoparticles containing immiscible metal elements. In other schemes, a sample is put into a high-temperature furnace for synthesis, and the method is difficult to obtain high-entropy alloy nanoparticles with single phase; therefore, it is difficult to realize the in-situ growth of the high-entropy alloy nanoparticles on the flexible substrate in the prior art so far.
Disclosure of Invention
In order to solve the technical problem, the invention discloses a method for growing high-entropy alloy nanoparticles on a flexible substrate, which comprises the following steps:
obtaining a flexible substrate;
growing a three-dimensional graphene film with a preset shape on the flexible substrate by adopting a laser direct writing technology;
obtaining a precursor solution of pre-synthesized high-entropy alloy nanoparticles;
dropwise adding the precursor solution to the three-dimensional graphene film to form a pretreated sample;
and carrying out radiation heating treatment on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology to obtain the high-entropy alloy nanoparticles.
Further, obtaining a precursor solution of the pre-synthesized high-entropy alloy nanoparticles, comprising:
determining target metal elements according to the pre-synthesized high-entropy alloy nanoparticles, wherein the target metal elements comprise at least five metal elements;
selecting precursors of metal salts corresponding to all metal elements; the chemical formula of the precursor of the metal salt comprises MClxHy, and M refers to a metal element;
and dissolving precursors of metal salts corresponding to the metal elements into a set solvent together to form a precursor solution of the pre-synthesized high-entropy alloy nano-particles.
Further, the target metal element includes at least five of Mn, Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, Ir, Pt, Au, Ce, or Sn elements.
Further, characterized in that the flexible substrate comprises a polyimide substrate or a flexible film coated with polyimide.
Further, in the step of carrying out radiation heating treatment on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology, the power of the infrared laser wavelength is 0.01-25W, the scanning speed is 0.01-100cm/s, and the wavelength is 9-11 μm.
Further, the structure of the high-entropy alloy nanoparticles is a face-centered cubic structure, and the size range of the high-entropy alloy nanoparticles is 1-100 nm.
By adopting the technical scheme, the invention has the following beneficial effects:
according to the method for growing the high-entropy alloy nanoparticles on the flexible substrate, the graphene film with the three-dimensional structure can be grown on the surface of the flexible substrate in situ by the laser direct writing technology, and the graphene film can be designed into a pattern meeting the requirements of a specific flexible electronic device according to the requirements; the metal salt precursor attached to the graphene carrier can be thermally desorbed by means of a laser direct writing technology, so that the in-situ growth of the high-entropy alloy nanoparticles is realized; the three-dimensional graphene is used as a carrier, so that the uniformity of the size of the high-entropy alloy nanoparticles and the total loading capacity of the alloy are improved; the laser direct writing technology can realize point-by-point scanning type radiant heating only on the graphene film area, so that high-temperature thermal damage to the flexible substrate is effectively avoided; meanwhile, the pulse laser pyrolysis growth mechanism is also beneficial to obtaining the high-entropy alloy nanoparticles with single phase.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for growing high-entropy alloy nanoparticles on a flexible substrate according to an embodiment of the present invention.
Fig. 2 is an XRD spectrum of a quinary high-entropy alloy (ptpdrhruiir) nanoparticle prepared by the method provided by the embodiment of the present invention.
Fig. 3 is an SEM topography of a nanofiber array of a three-dimensional graphene film grown in situ on a polyimide substrate according to an embodiment of the present invention and a TEM topography of a single graphene nanofiber modified by a quinary high-entropy alloy (ptaadpdrhruri) nanoparticle.
Fig. 4 is a TEM topography of eight-element high entropy alloy (PtPdRhRuIrCeAuCu) nanoparticles grown on a three-dimensional graphene film of a polyimide substrate according to an embodiment of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. In the description of the embodiments of the present invention, it should be understood that the terms "upper", "lower", "top", "bottom", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only used for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Moreover, the terms "first," "second," and the like are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein.
Referring to fig. 1, fig. 1 is a schematic flow chart of a method for growing high-entropy alloy nanoparticles on a flexible substrate according to an embodiment of the present invention; the method may comprise the steps of:
s101, obtaining a flexible substrate; in an embodiment of the present invention, the flexible substrate may include a polyimide substrate or a flexible film coated with polyimide.
S102, growing a three-dimensional graphene film with a preset shape on the flexible substrate by adopting a laser direct writing technology; the shape of the three-dimensional graphene film can be set according to the requirements of flexible electronic devices.
S103, obtaining a precursor solution of the pre-synthesized high-entropy alloy nanoparticles;
the method comprises the following steps of (1) obtaining a precursor solution of the high-entropy alloy nanoparticles, wherein the precursor solution can comprise;
determining target metal elements according to the pre-synthesized high-entropy alloy nanoparticles, wherein the target metal elements comprise at least five metal elements; it may be practiced that the target metal element may include five to fourteen metal elements;
selecting precursors of metal salts corresponding to all metal elements according to target metals; wherein, the chemical formula of the precursor of the metal salt can be MClxHy, M refers to metal elements, and can comprise manganese Mn, cobalt Co, nickel Ni, copper Cu, zinc Zn, ruthenium Ru, rhodium Rh, palladium Pd, iridium Ir, platinum Pt, gold Au, cerium Ce or tin Sn and other elements; it is practicable that the chemical formula of the precursor of the metal salt may be MClx, for example, when M is Fe element;
and dissolving precursors of metal salts corresponding to the metal elements into a set solvent together to form a precursor solution of the pre-synthesized high-entropy alloy nano-particles. In an embodiment of the present invention, the target metal element includes at least five of Mn, Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, Ir, Pt, Au, Ce, or Sn elements.
In the embodiment of the invention, the concentration of the precursor solution of the pre-synthesized high-entropy alloy nanoparticles can be 1 mM-1M; the set solvent may include a combination of one or more of water, methanol, ethanol, or isopropanol.
S104, dropwise adding the precursor solution to the three-dimensional graphene film to form a pretreated sample; in the embodiment of the invention, the precursor solution can be uniformly dripped on the three-dimensional graphene film.
And S105, carrying out radiation heating treatment on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology to obtain the high-entropy alloy nanoparticles.
In the embodiment of the invention, the laser direct writing technology is adopted to carry out radiation heating treatment on the three-dimensional graphene film on the pretreated sample to obtain high-entropy alloy nanoparticles; the method can comprise the following steps:
placing the pre-treated sample into a chamber; the cavity is provided with a zinc selenide window;
closing the cavity;
introducing inert gas into the cavity for purging for a set time to remove O adsorbed on the surface of the pretreated sample 2 And H 2 O steam;
and (3) carrying out radiant heating on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology through the zinc selenide window, so that the metal salt is subjected to rapid thermal decomposition, and the high-entropy alloy nano particles are obtained by reduction.
In the embodiment of the invention, in the step of performing radiant heating treatment on the three-dimensional graphene film on the pretreated sample by using the laser direct writing technology, the wavelength of infrared laser is 9-11 μm, optionally, the wavelength of infrared laser can be 9.3 μm, 10.2 μm or 10.6 μm, the power can be 0.01-25W, and the scanning speed can be 0.01-100 cm/s. The growth dynamics process of the high-entropy alloy nanoparticles can be effectively controlled through infrared laser parameters (such as power, scanning speed and the like), so that the size, density, uniformity and the like of the high-entropy alloy nanoparticles can be effectively regulated and controlled according to actual requirements;
in an embodiment of the present invention, before the step of performing the radiant heating treatment on the three-dimensional graphene film on the pretreated sample by using the laser direct writing technology, the method further includes:
and drying the pretreated sample.
In the embodiment of the invention, the pretreatment sample is dried; the method can comprise the following steps:
placing the pretreated sample in a vacuum oven for drying or blowing the pretreated sample by inert gas;
the setting temperature of the vacuum oven can be 60-120 ℃, and the inert gas can comprise Ar or N 2 。
In the embodiment of the invention, the structure of the high-entropy alloy nanoparticles is a face-centered cubic structure, and the size range of the high-entropy alloy nanoparticles is 1-100 nm.
FIG. 2 is a diffraction of X-rays (XRD) spectrum of a five-membered high entropy alloy (PtPdRhRuIr) nanoparticle with a face centered cubic structure prepared by using polyimide as a flexible substrate and Pt, Pd, Rh, Ru and Ir as target metal elements, wherein the abscissa is the angle of a diffraction angle and the ordinate is the intensity of a diffraction peak; according to XRD patterns, the synthesized high-entropy alloy nanoparticles have a face-centered cubic structure and do not contain impurity phases.
Fig. 3 is a Scanning Electron Microscope (SEM) morphology of a nanofiber array of a three-dimensional graphene thin film grown in situ on a polyimide substrate (left image) and a Transmission Electron Microscope (TEM) morphology of single graphene nanofiber modified with a five-element high entropy alloy (ptaadpdrhrhrhruri) nanoparticle (right image). According to an SEM image, the graphene nanofiber array grows perpendicular to the polyimide film, has good bonding performance with the substrate, and is beneficial to improving the uniformity of the size of the high-entropy alloy nanoparticles.
Fig. 4 is a TEM topography of eight-element high-entropy alloy (PtPdRhRuIrCeAuCu) nanoparticles grown on a three-dimensional graphene film of a polyimide substrate, and it can be known from the TEM topography that the high-entropy alloy nanoparticles are uniformly distributed on the three-dimensional graphene film and have good uniformity of size.
According to the method for growing the high-entropy alloy nanoparticles on the flexible substrate, provided by the embodiment of the invention, a layer of graphene film with a three-dimensional structure can be grown on the surface of the flexible substrate in situ by a laser direct writing technology, and a pattern meeting the requirements of a specific flexible electronic device can be designed according to the requirements; the metal salt precursor attached to the graphene carrier can be thermally desorbed by means of a laser direct writing technology, so that the in-situ growth of the high-entropy alloy nanoparticles is realized; the three-dimensional graphene is used as a carrier, so that the uniformity of the size of the high-entropy alloy nanoparticles and the total loading capacity of the alloy are improved; the laser direct writing technology can realize point-by-point scanning type radiant heating only on the graphene film area, so that high-temperature thermal damage to the flexible substrate is effectively avoided; meanwhile, the pulse laser pyrolysis growth mechanism is also beneficial to obtaining the high-entropy alloy nanoparticles with single phase.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for growing high-entropy alloy nanoparticles on a flexible substrate is characterized by comprising the following steps:
obtaining a flexible substrate;
growing a three-dimensional graphene film with a preset shape on the flexible substrate by adopting a laser direct writing technology;
obtaining a precursor solution of pre-synthesized high-entropy alloy nanoparticles;
dropwise adding the precursor solution to the three-dimensional graphene film to form a pretreated sample;
and carrying out radiation heating treatment on the three-dimensional graphene film on the pretreated sample by adopting a laser direct writing technology to obtain the high-entropy alloy nanoparticles.
2. A method for growing high-entropy alloy nanoparticles on a flexible substrate according to claim 1, wherein the obtaining of a precursor solution of pre-synthesized high-entropy alloy nanoparticles comprises:
determining target metal elements according to the pre-synthesized high-entropy alloy nanoparticles, wherein the target metal elements comprise at least five metal elements;
selecting precursors of metal salts corresponding to all metal elements; the chemical formula of the precursor of the metal salt comprises MClxHy, and M refers to a metal element;
and dissolving precursors of metal salts corresponding to the metal elements into a set solvent together to form a precursor solution of the pre-synthesized high-entropy alloy nano-particles.
3. A method for growing high entropy alloy nanoparticles on a flexible substrate as claimed in claim 2, wherein the target metal elements include at least five of Mn, Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, Ir, Pt, Au, Ce or Sn elements.
4. A method for growing high entropy alloy nanoparticles on a flexible substrate according to claim 1, wherein the flexible substrate comprises a polyimide substrate or a flexible film coated with polyimide.
5. A method for growing high-entropy alloy nanoparticles on a flexible substrate according to claim 1, wherein in the step of performing radiant heating treatment on the three-dimensional graphene film on the preprocessed sample by using a laser direct writing technology, the power of an infrared laser is 0.01-25W, the scanning speed is 0.01-100cm/s, and the wavelength is 9-11 μm.
6. A method for growing high-entropy alloy nanoparticles on a flexible substrate according to claim 1, wherein the structure of the high-entropy alloy nanoparticles is a face-centered cubic structure, and the size of the high-entropy alloy nanoparticles is in the range of 1-100 nm.
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