CN108505023B - Preparation method of self-supporting two-dimensional metal film welded by using protein - Google Patents
Preparation method of self-supporting two-dimensional metal film welded by using protein Download PDFInfo
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- CN108505023B CN108505023B CN201810458256.5A CN201810458256A CN108505023B CN 108505023 B CN108505023 B CN 108505023B CN 201810458256 A CN201810458256 A CN 201810458256A CN 108505023 B CN108505023 B CN 108505023B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/16—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 by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of a self-supporting two-dimensional metal film welded by using protein, which utilizes self-assembly of metal nanoparticles formed by in-situ reduction of metal ions by using protein (lysozyme, albumin, α -amylase, collagen, keratin, pepsin, bovine serum albumin and the like) to induce a reducing agent to self-assemble at a gas-liquid interface to form the self-supporting two-dimensional metal film welded by using protein.
Description
Technical Field
The invention belongs to the technical field of metal film preparation, and particularly relates to a preparation method of a self-supporting two-dimensional metal film by using protein welding.
Background
With the rapid development of the nano science technology, the research focus of the nano science has been developed from the basic synthesis and characterization of materials and structures to the application-oriented system integration and device functionalization. The independent and disordered low-dimensional nano material is taken as a building unit, and the construction of a functional two-dimensional structure film or device from bottom to top is an important development direction.
Metals are an important class of materials with a wide range of practical applications, and their properties are closely related to their size and morphology. Self-supporting metal films of several tens to several hundreds of nanometers in thickness have unusual physical and chemical properties due to strong quantum confinement and surface effects. The flexible and bendable metal nano film with high conductivity is a novel nano functional material and has wide application in the aspects of transparent conductive electrodes, chemical sensors, catalysis, photoelectric devices and the like.
At present, the conductive metal film is generally processed by a vacuum vapor deposition method (such as sputtering, electron beam evaporation, molecular beam epitaxy, and the like), and can also be prepared from chemically synthesized metal nanoparticles by a solution processing method (such as self-assembly, spin coating, drop coating, L B film deposition, and the like).
Disclosure of Invention
The invention aims to provide a method for preparing a self-supporting two-dimensional metal film by using protein welding metal nanoparticles.
Aiming at the purposes, the technical scheme adopted by the invention is that a heavy metal salt solution is added into a 0.02-10 mg/m L protein aqueous solution, and a reducing agent is added to reduce heavy metal ions into simple substances, namely a layer of self-supporting two-dimensional metal film welded by protein is formed on the surface of the solution.
The metal salt solution is at least one of silver ammonia solution, silver nitrate aqueous solution, chloroplatinic acid aqueous solution, chloroauric acid aqueous solution and copper sulfate pentahydrate aqueous solution, and the protein is any one of lysozyme, albumin, α -amylase, collagen, keratin, pepsin and bovine serum albumin.
When the metal salt solution is a silver ammonia solution, preferably, 10-30 mg/m L silver ammonia solution, 0.02-10 mg/m L protein aqueous solution and 10-30 mg/m L glucose aqueous solution are uniformly mixed in equal volume, and the mixture is stood at room temperature for 2-9 hours, so that a layer of protein-welded self-supporting two-dimensional silver film is formed on the surface of the solution.
When the metal salt solution is a chloroauric acid aqueous solution, preferably mixing 4-5 mg/m L chloroauric acid aqueous solution, 5-10 mg/m L protein aqueous solution and 4-5 mg/m L sodium citrate dihydrate aqueous solution in equal volume, standing at 35-40 ℃ for 24-48 hours, and forming a layer of protein-welded self-supporting two-dimensional gold film on the surface of the solution.
When the metal salt solution is a copper sulfate pentahydrate aqueous solution, preferably, 20-30 mg/m L copper sulfate pentahydrate aqueous solution, 5-10 mg/m L protein aqueous solution and 40-50 mg/m L vitamin C aqueous solution are uniformly mixed in equal volume, and the mixture is kept stand at 70-80 ℃ for 10-15 hours, so that a layer of self-supporting two-dimensional copper film welded by protein is formed on the surface of the solution.
When the metal salt solution is a chloroplatinic acid aqueous solution, preferably mixing 4-5 mg/m L chloroplatinic acid aqueous solution, 2-5 mg/m L protein aqueous solution and 10-30 mg/m L vitamin C aqueous solution in equal volume uniformly, and standing at room temperature for 12-24 hours to form a layer of protein-welded self-supporting two-dimensional platinum film on the surface of the solution.
When the metal salt solution is a silver nitrate aqueous solution and a chloroauric acid aqueous solution, preferably mixing 10-30 mg/m L silver nitrate aqueous solution, 4-5 mg/m L chloroauric acid aqueous solution, 2-5 mg/m L protein aqueous solution and 10-30 mg/m L glucose aqueous solution in equal volume, standing at room temperature for 12-24 hours, and forming a layer of self-supporting two-dimensional gold-silver alloy film welded by protein on the surface of the solution.
The invention has the following beneficial effects:
1. the invention utilizes the self-assembly of metal nano particles formed by reducing metal ions in situ by a protein-induced reducing agent on a gas-liquid interface to form a self-supporting two-dimensional metal film welded by protein, wherein the thickness of the silver film is about 20-200 nm, the reflectivity is about 20-80%, and the silver content is about 75-98%.
2. The preparation method of the self-supporting two-dimensional metal film welded by the protein is simple and environment-friendly, and has wide application prospect in the field of flexible electronic devices based on excellent conductive performance of the metal film.
Drawings
FIG. 1 is a photograph of lysozyme welded self-supporting two-dimensional silver film having high reflective properties prepared in example 1.
FIG. 2 is an atomic force microscope image of a lysozyme welded self-supporting two-dimensional silver film having high reflective properties prepared in example 1.
FIG. 3 is a photograph of lysozyme welded self-supporting two-dimensional silver film having high electrical conductivity prepared in example 3.
FIG. 4 is a cold field scanning electron micrograph of a lysozyme welded self-supporting two-dimensional silver film having high electrical conductivity prepared in example 3.
FIG. 5 is a graph of current versus time for a lysozyme welded, self-supporting two-dimensional silver film having high electrical conductivity prepared in example 3.
FIG. 6 is a cold field scanning electron micrograph of a albumin-welded self-supporting two-dimensional silver film prepared according to example 5.
FIG. 7 is a cold field scanning electron micrograph of α -amylase welded two-dimensional silver film prepared according to example 6.
FIG. 8 is a cold field scanning electron micrograph of a collagen-welded two-dimensional silver film prepared according to example 7.
FIG. 9 is a cold field scanning electron micrograph of a keratin-welded two-dimensional silver film prepared according to example 8.
FIG. 10 is a cold field scanning electron micrograph of a pepsin welded two-dimensional silver film prepared in example 9.
FIG. 11 is a scanning electron micrograph of a BSA welded two-dimensional silver film prepared in example 10.
FIG. 12 is a cold field scanning electron micrograph of a lysozyme welded two-dimensional gold film prepared in example 11.
FIG. 13 is a cold field scanning electron micrograph of a lysozyme welded two-dimensional copper film made in example 12.
FIG. 14 is a cold field scanning electron micrograph of a lysozyme welded two-dimensional platinum film made in example 13.
FIG. 15 is a scanning electron micrograph of a lysozyme-welded two-dimensional gold-silver alloy thin film prepared in example 14 in a cold field.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
The preparation method comprises the steps of adding 20mg of lysozyme into 10m L of ultrapure water to prepare a lysozyme aqueous solution of 2mg/m L, adding 0.3g of D-glucose into 10m L0 of ultrapure water to prepare a D-glucose aqueous solution of 30mg/m L1, adding 0.3g of silver nitrate into 2.5m L2 of ultrapure water to prepare a silver nitrate aqueous solution of 120mg/m L3, adding 2.5m L5120 mg/m L6 of the silver nitrate solution into a 15m L4 PE tube, then adding ammonia water dropwise, oscillating while dropping until the initially generated precipitate is just dissolved, fixing the volume to 10m L to obtain a silver-ammonia solution of 30mg/m L, forming a lysozyme aqueous solution of 10m L2 mg/m L, forming a layer of D-glucose aqueous solution of 10m L30 mg/m L and a silver-ammonia solution of 10m L30 mg/m L, standing for 3 hours, welding a layer of a two-dimensional silver-supported film on the surface, and obtaining a silver-based on a silver-supported film with a silver-based on a silver-supported film reflection graph showing that the content of about 50 nm silver-loaded lysozyme film.
Example 2
In this example, the lysozyme aqueous solution of 2mg/m L in example 1 was replaced by the lysozyme aqueous solution of 0.5mg/m L with the same volume, and the other steps were the same as in example 1, and a lysozyme welded self-supporting two-dimensional silver film with a silver content of about 90% was formed on the surface of the mixed solution.
Example 3
In this example, the lysozyme aqueous solution of 2mg/m L in example 1 was replaced with the lysozyme aqueous solution of 0.2mg/m L in the same volume, and a lysozyme-welded self-supporting two-dimensional silver film (see fig. 3 and 4) having a silver content of about 98% was formed on the surface of the mixed solution in the same manner as in example 1, as can be seen from fig. 5, which had excellent conductivity.
Example 4
In the embodiment, the lysozyme aqueous solution of 2mg/m L in the embodiment 1 is replaced by the lysozyme aqueous solution of 0.02mg/m L with the same volume, the standing time at room temperature is shortened to 2 hours, other steps are the same as the embodiment 1, a layer of lysozyme welded self-supporting two-dimensional silver film is formed on the surface of the mixed solution, and the silver content is about 99 percent.
Example 5
In this example, the 2mg/m L aqueous lysozyme solution in example 1 was replaced with an equal volume of 2mg/m L aqueous albumin solution, and the other steps were the same as in example 1, to form a albumin-welded self-supporting two-dimensional silver film (see FIG. 6) having high reflectivity on the surface of the mixed solution.
Example 6
In this example, the 2mg/m L aqueous lysozyme solution in example 1 was replaced with an equal volume of 2mg/m L aqueous α -amylase solution, and a α -amylase-welded self-supporting two-dimensional silver film (see FIG. 7) having high reflectivity was formed on the surface of the mixed solution in the same manner as in example 1.
Example 7
In this example, the 2mg/m L aqueous lysozyme solution in example 1 was replaced with an equal volume of 2mg/m L aqueous collagen solution, and the procedure was the same as in example 1, and a collagen-welded self-supporting two-dimensional silver film (see FIG. 8) having high reflectivity was formed on the surface of the mixed solution.
Example 8
In this example, the aqueous solution of lysozyme at 2mg/m L in example 1 was replaced with an equal volume of 2mg/m L aqueous solution of keratin, and the procedure was the same as in example 1, and a keratin-welded self-supporting two-dimensional silver film (see FIG. 9) having high reflectivity was formed on the surface of the mixed solution.
Example 9
In this example, the aqueous solution of lysozyme at 2mg/m L in example 1 was replaced with an equal volume of aqueous solution of pepsin at 2mg/m L, and the other steps were the same as in example 1, and a self-supporting two-dimensional silver film (see FIG. 10) welded with pepsin was formed on the surface of the mixed solution, which had high reflectivity.
Example 10
In this example, 2mg/m L of the aqueous lysozyme solution of example 1 was replaced with an equal volume of 2mg/m L aqueous bovine serum albumin solution, and the other steps were the same as in example 1, whereby a layer of bovine serum albumin welded self-supporting two-dimensional silver film (see fig. 11) was formed on the surface of the mixed solution, which was highly reflective.
Example 11
Adding 50mg of lysozyme into 10m L ultrapure water to prepare a lysozyme aqueous solution with a concentration of 5mg/m L, adding 40mg of chloroauric acid into 10m L0 ultrapure water to prepare a chloroauric acid aqueous solution with a concentration of 4mg/m L1, adding 40mg of sodium citrate dihydrate into 10m L ultrapure water to prepare a sodium citrate dihydrate aqueous solution with a concentration of 4mg/m L, uniformly mixing the lysozyme aqueous solution with a concentration of 10m L5 mg/m L, the chloroauric acid aqueous solution with a concentration of 10m L4 mg/m L and the sodium citrate dihydrate aqueous solution with a concentration of 10m L4 mg/m L, standing at 37 ℃ for 48 hours to form a layer of lysozyme welded self-supporting two-dimensional gold film on the surface of the mixed solution (see figure 12), wherein the obtained gold film is wine red and is assembled by lysozyme welded gold nanoparticles.
Example 12
Adding 50mg of lysozyme into 10m L ultrapure water to prepare a lysozyme aqueous solution with a concentration of 5mg/m L, adding 250mg of blue vitriol into 10m L0 ultrapure water to prepare a copper sulfate aqueous solution with a concentration of 25mg/m L1, adding 430mg of vitamin C into 10m L ultrapure water to prepare a vitamin C aqueous solution with a concentration of 43mg/m L, uniformly mixing 10m L5 mg/m L lysozyme aqueous solution, 10m L25 mg/m L copper sulfate aqueous solution and 10m L43 mg/m L vitamin C aqueous solution, standing at 80 ℃ for 12 hours, forming a layer of lysozyme welded self-supporting two-dimensional copper film (shown in figure 13) on the surface of the mixed solution, wherein the obtained copper film is brown and is assembled by lysozyme welded copper nanoparticles.
Example 13
Adding 50mg of lysozyme into 10m L ultrapure water to prepare a lysozyme aqueous solution with a concentration of 5mg/m L, adding 40mg of chloroplatinic acid into 10m L0 ultrapure water to prepare a chloroplatinic acid aqueous solution with a concentration of 4mg/m L1, adding 300mg of vitamin C into 10m L ultrapure water to prepare a vitamin C aqueous solution with a concentration of 30mg/m L, uniformly mixing 10m L5 mg/m L lysozyme aqueous solution, 10m L4 mg/m L chloroplatinic acid aqueous solution and 10m L30 mg/m L vitamin C aqueous solution, standing at room temperature for 12 hours to form a layer of lysozyme-welded self-supporting two-dimensional platinum film (shown in figure 14) on the surface of the mixed solution, wherein the obtained platinum film is gray black and is assembled by lysozyme welding platinum nanoparticles.
Example 14
Adding 50mg of lysozyme into 10m L ultrapure water to prepare a lysozyme aqueous solution with a concentration of 5mg/m L, adding 40mg of chloroauric acid into 10m L0 ultrapure water to prepare a chloroauric acid aqueous solution with a concentration of 4mg/m L1, adding 300mg of silver nitrate into 10m L2 ultrapure water to prepare a silver nitrate aqueous solution with a concentration of 30mg/m L3, adding 300mg of D-glucose into 10m L4 ultrapure water to prepare a D-glucose aqueous solution with a concentration of 30mg/m L5, uniformly mixing 10m L5 mg/m L of the lysozyme aqueous solution, 10m L4 mg/m L of the chloroauric acid aqueous solution, 10m L30 mg/m L of the silver nitrate aqueous solution and 10m L30 mg/m L of the D-glucose aqueous solution, standing at room temperature for 12 hours to form a layer of a self-supporting gold-silver alloy film welded with lysozyme on the surface (see figure 15), wherein the obtained gold-silver alloy film is in a brown green color, and gold-silver alloy nano particles are assembled by welding.
Claims (6)
1. A preparation method of a self-supporting two-dimensional metal film welded by using protein is characterized in that a heavy metal salt solution is added into a 0.02-10 mg/m L protein aqueous solution, and a reducing agent is added to reduce heavy metal ions into simple substances, so that a layer of self-supporting two-dimensional metal film welded by using protein is formed on the surface of the solution;
the protein is any one of lysozyme, albumin, α -amylase, collagen, keratin, gastric protein and bovine serum albumin;
the metal salt solution is at least one of silver ammonia solution, silver nitrate aqueous solution, chloroplatinic acid aqueous solution, chloroauric acid aqueous solution and copper sulfate pentahydrate aqueous solution.
2. The method for preparing a self-supporting two-dimensional metal film by protein soldering as claimed in claim 1, wherein when the metal salt solution is a silver ammonia solution, the silver ammonia solution of 10-30 mg/m L, the protein aqueous solution of 0.02-10 mg/m L and the glucose aqueous solution of 10-30 mg/m L are uniformly mixed in equal volume, and the mixture is allowed to stand at room temperature for 2-9 hours to form a layer of self-supporting two-dimensional silver film by protein soldering on the surface of the solution.
3. The method for preparing a self-supporting two-dimensional metal film by protein welding according to claim 1, wherein when the metal salt solution is an aqueous solution of chloroauric acid, a layer of self-supporting two-dimensional gold film by protein welding is formed on the surface of the solution by uniformly mixing an aqueous solution of chloroauric acid of 4-5 mg/m L, an aqueous solution of protein of L of-10 mg/m, and an aqueous solution of sodium citrate dihydrate of 4-5 mg/m L in equal volumes, and standing the mixture at 35-40 ℃ for 24-48 hours.
4. The method for preparing a self-supporting two-dimensional metal film by protein welding as claimed in claim 1, wherein when the metal salt solution is copper sulfate pentahydrate aqueous solution, 20-30 mg/m L copper sulfate pentahydrate aqueous solution, 5-10 mg/m L protein aqueous solution, 40-50 mg/m L vitamin C aqueous solution are uniformly mixed in equal volume, and the mixture is left to stand at 70-80 ℃ for 10-15 hours to form a layer of self-supporting two-dimensional copper film by protein welding on the surface of the solution.
5. The method for preparing a self-supporting two-dimensional metal film by protein welding according to claim 1, wherein when the metal salt solution is an aqueous solution of chloroplatinic acid, a layer of self-supporting two-dimensional platinum film by protein welding is formed on the surface of the solution by uniformly mixing an aqueous solution of 4-5 mg/m L chloroplatinic acid with an aqueous solution of 2-5 mg/m L protein and an aqueous solution of 10-30 mg/m L vitamin C in equal volume, and standing at room temperature for 12-24 hours.
6. The method for preparing a self-supporting two-dimensional metal film by protein welding according to claim 1, wherein when the metal salt solution is a silver nitrate aqueous solution and a chloroauric acid aqueous solution, a silver nitrate aqueous solution of 10-30 mg/m L, a chloroauric acid aqueous solution of 4-5 mg/m L, a protein aqueous solution of 2-5 mg/m L, and a glucose aqueous solution of 10-30 mg/m L are uniformly mixed in equal volumes, and then the mixture is allowed to stand at room temperature for 12-24 hours, so that a layer of the self-supporting two-dimensional gold-silver alloy film welded by protein is formed on the surface of the solution.
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