CN108505023A - A kind of preparation method of self-supporting two-dimensional metallic film using protein welding - Google Patents
A kind of preparation method of self-supporting two-dimensional metallic film using protein welding Download PDFInfo
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- CN108505023A CN108505023A CN201810458256.5A CN201810458256A CN108505023A CN 108505023 A CN108505023 A CN 108505023A CN 201810458256 A CN201810458256 A CN 201810458256A CN 108505023 A CN108505023 A CN 108505023A
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Abstract
The invention discloses a kind of preparation methods of the self-supporting two-dimensional metallic film using protein welding, the metal nanoparticle that this method is formed using protein (lysozyme, albumin, alpha amylase, collagen, keratin, stomach cardia, bovine serum albumin(BSA) etc.) induction reducing agent in-situ reducing metal ion forms the self-supporting two-dimensional metallic film of protein welding in gas-liquid interface self assembly.Preparation method of the present invention is simple, environmental-friendly, is applicable in films such as gold, silver, platinum, copper and electrums, and gained metal film has excellent electric conductivity or high reflectivity, has broad application prospects in flexible electronic device and optical device field.
Description
Technical field
The invention belongs to the preparing technical fields of metallic film, and in particular to a kind of self-supporting two welded using protein
Tie up the preparation method of metallic film.
Background technology
With the rapid development of nanoscale science and technology, the research emphasis of nano science from basis " material and structure
Synthesis, characterization " develops to application oriented " system integration and device function " direction.With independent, unordered low-dimensional nanometer material
Material is building " unit ", and it is exactly one of important development side to construct functional two-dimensional structure film or device from bottom to top
To.
Metal is a kind of important material, has an extensive practical application, their property and their size, form are close
Cut phase is closed.Due to strong quantum confinement and skin effect, the self-supporting metal film of tens to hundreds of nanometers thickness, which has, not to be sought
Normal physics and chemical characteristic.Metal nanometer thin film with highly conductive characteristic, flexible is a kind of novel nanometer work(
Energy material, it has extensive use in transparent conductive electrode, chemical sensor, catalysis and photoelectric device etc..
Currently, conductive metal film generally use vacuum vapor deposition (such as sputtering, electron beam evaporation, molecular beam epitaxy)
Method is processed, and the method (such as self assembly, spin coating, drop coating, LB films deposition) of solution processing can also be used by chemically synthesized gold
Belong to nano-particle to be prepared.Vacuum-deposited method needs expensive large-scale instrument, processing cost higher.Although with solution
Processing method cost is relatively low, but the metallic in film is often unordered stacking states, there are a large amount of particle intervals, thus
Influence the ability that metallic film transmits electronics.Develop the metal nanometer thin film material of solution processable and can neatly regulate and control it
Multiple performance including electric conductivity by the manufacturing cost that can reduce metallic film but also promotes it to be answered various
With.
Invention content
The purpose of the present invention is to provide a kind of self-supporting two-dimensional metallic is prepared using protein welding metal nano particle
The method of film.
For above-mentioned purpose, the technical solution adopted in the present invention is:0.02~10mg/mL is added in heavy metallic salt solution
In protein aqueous solution, and reducing agent, which is added, makes heavy metal ion be reduced into simple substance, i.e., forms one layer of protein in solution surface
The self-supporting two-dimensional metallic film of welding.
Above-mentioned metal salt solution is silver ammino solution, silver nitrate aqueous solution, chloroplatinic acid aqueous solution, aqueous solution of chloraurate, five
At least one of brochanite aqueous solution, protein are lysozyme, albumin, alpha-amylase, collagen, keratin, stomach egg
In vain, any one in bovine serum albumin(BSA).
When the metal salt solution is silver ammino solution, preferably by the silver ammino solution of 10~30mg/mL and 0.02~10mg/
ML protein aqueous solutions, 10~30mg/mL glucose solution be uniformly mixed in equal volume, be stored at room temperature 2~9 hours, that is, exist
Solution surface forms the self-supporting two dimension Ag films of one layer of protein welding.
When the metal salt solution is aqueous solution of chloraurate, preferably by 4~5mg/mL aqueous solution of chloraurate and 5~
10mg/mL protein aqueous solutions, 4~5mg/mL citrate dihydrate sodium water solutions are uniformly mixed in equal volume, and 35~40 DEG C stand 24
~48 hours, i.e., the self-supporting two dimension gold thin film of one layer of protein welding is formed in solution surface.
It is preferably that 20~30mg/mL cupric sulfate pentahydrates is water-soluble when the metal salt solution is cupric sulfate pentahydrate aqueous solution
Liquid is uniformly mixed in equal volume with 5~10mg/mL protein aqueous solutions, 40~50mg/mL vitamin Cs aqueous solution, and 70~80 DEG C quiet
It sets 10~15 hours, i.e., forms the self-supporting two dimension Copper thin film of one layer of protein welding in solution surface.
When the metal salt solution is chloroplatinic acid aqueous solution, preferably by 4~5mg/mL chloroplatinic acid aqueous solutions and 2~5mg/
ML protein aqueous solutions, 10~30mg/mL vitamin C aqueous solution be uniformly mixed in equal volume, be stored at room temperature 12~24 hours, i.e.,
The self-supporting two dimension platinum film of one layer of protein welding is formed in solution surface.
When the metal salt solution is silver nitrate aqueous solution and aqueous solution of chloraurate, preferably by 10~30mg/mL nitric acid
Silver-colored aqueous solution, 4~5mg/mL aqueous solution of chloraurate, 2~5mg/mL protein aqueous solutions, 10~30mg/mL glucose solutions
It is isometric to be uniformly mixed, it is stored at room temperature 12~24 hours, i.e., forms the self-supporting two dimension of one layer of protein welding in solution surface
Electrum film.
Beneficial effects of the present invention are as follows:
1, the metal nanoparticle that the present invention is formed using protein induction reducing agent in-situ reducing metal ion is in gas-liquid
Interface self assembly forms the self-supporting two-dimensional metallic film of protein welding, and the thickness of wherein Ag films is about 20~200nm,
Reflectivity is about 20%~80%, and silver content is about 75%~98%, can synthesize high reflectivity silverskin through the invention and height is led
Electrical silverskin.
2, the preparation method of the self-supporting two-dimensional metallic film of present protein welding is simple, environmental-friendly, based on gold
Belong to the excellent electric conductivity of film, has broad application prospects in flexible electronic device field.
Description of the drawings
Fig. 1 is the self-supporting two dimension Ag films photo of the lysozyme welding with high reflection property prepared by embodiment 1.
Fig. 2 is the atom of the self-supporting two dimension Ag films of the lysozyme welding with high reflection property prepared by embodiment 1
Force microscope figure.
Fig. 3 is the self-supporting two dimension Ag films photo of the lysozyme welding with high conduction performance prepared by embodiment 3.
Fig. 4 is the awkward silence at a meeting of the self-supporting two dimension Ag films of the lysozyme welding with high conduction performance prepared by embodiment 3
Scanning electron microscope (SEM) photograph.
Fig. 5 is the electric current-of the self-supporting two dimension Ag films of the lysozyme welding with high conduction performance prepared by embodiment 3
Time plot.
Fig. 6 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the self-supporting two dimension Ag films of albumin welding prepared by embodiment 5.
Fig. 7 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Ag films of alpha-amylase welding prepared by embodiment 6.
Fig. 8 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Ag films of collagen welding prepared by embodiment 7.
Fig. 9 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Ag films of keratin welding prepared by embodiment 8.
Figure 10 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Ag films of stomach cardia welding prepared by embodiment 9.
Figure 11 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Ag films of bovine serum albumin(BSA) welding prepared by embodiment 10.
Figure 12 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional gold thin film of lysozyme welding prepared by embodiment 11.
Figure 13 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional Copper thin film of lysozyme welding prepared by embodiment 12.
Figure 14 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimentional platinum film of lysozyme welding prepared by embodiment 13.
Figure 15 is the awkward silence at a meeting scanning electron microscope (SEM) photograph of the two-dimensional gold silver alloy film of lysozyme welding prepared by embodiment 14.
Specific implementation mode
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
20mg lysozymes are added in 10mL ultra-pure waters, the Lysozyme in Aqueous Solution of 2mg/mL is configured to;By 0.3gD- grapes
Sugar is added in 10mL ultra-pure waters, is configured to the D-Glucose aqueous solution of 30mg/mL;2.5mL ultra-pure waters are added in 0.3g silver nitrates
In, it is configured to the silver nitrate aqueous solution of 120mg/mL;The silver nitrate solution of 2.5mL 120mg/mL is added in 15mL PE pipes,
Then ammonium hydroxide is added dropwise, is vibrated in drop, until the precipitation initially generated just dissolves, constant volume 10mL is obtained
The silver ammino solution of 30mg/mL;By the Lysozyme in Aqueous Solution of 10mL 2mg/mL, 10mL 30mg/mL D-Glucose aqueous solution with
The silver ammino solution of 10mL 30mg/mL is uniformly mixed, and is stored at room temperature 3 hours, forms what one layer of lysozyme welded on mixed liquor surface
Self-supporting two dimension Ag films, silver content are about 82%.Fig. 1 is as it can be seen that gained Ag films have high reflectivity, from Figure 2 it can be seen that should
The silver nano-grain that film is welded 50 ± 10nm or so by lysozyme assembles.
Embodiment 2
In the present embodiment, with the lysozyme of 2mg/mL in the Lysozyme in Aqueous Solution alternative embodiment 1 of isometric 0.5mg/mL
Aqueous solution, other steps are same as Example 1, and the self-supporting two dimension silver that one layer of lysozyme welding is formed on mixed liquor surface is thin
Film, silver content are about 90%.
Embodiment 3
In the present embodiment, with the lysozyme of 2mg/mL in the Lysozyme in Aqueous Solution alternative embodiment 1 of isometric 0.2mg/mL
Aqueous solution, other steps are same as Example 1, and the self-supporting two dimension Ag films of one layer of lysozyme welding are formed on mixed liquor surface
(see Fig. 3 and Fig. 4), silver content are about 98%.As seen from Figure 5, which has excellent electric conductivity.
Embodiment 4
In the present embodiment, with the lysozyme of 2mg/mL in the Lysozyme in Aqueous Solution alternative embodiment 1 of isometric 0.02mg/mL
Aqueous solution, being stored at room temperature the time foreshortens to 2 hours, other steps are same as Example 1, and one layer of bacteriolyze is formed on mixed liquor surface
The self-supporting two dimension Ag films of enzyme welding, silver content is about 99%.
Embodiment 5
In the present embodiment, with the lysozyme water of 2mg/mL in the albumin aqueous solution alternative embodiment 1 of isometric 2mg/mL
Solution, other steps are same as Example 1, and the self-supporting two dimension Ag films of one layer of albumin welding are formed on mixed liquor surface
(see Fig. 6), with high reflectivity.
Embodiment 6
In the present embodiment, with the lysozyme of 2mg/mL in the alpha-amylase aqueous solution alternative embodiment 1 of isometric 2mg/mL
Aqueous solution, other steps are same as Example 1, and the self-supporting two dimension silver that one layer of alpha-amylase welding is formed on mixed liquor surface is thin
Film (see Fig. 7), with high reflectivity.
Embodiment 7
In the present embodiment, with the lysozyme of 2mg/mL in the collagen aqueous solution alternative embodiment 1 of isometric 2mg/mL
Aqueous solution, other steps are same as Example 1, and the self-supporting two dimension silver that one layer of collagen welding is formed on mixed liquor surface is thin
Film (see Fig. 8), with high reflectivity.
Embodiment 8
In the present embodiment, with the lysozyme water of 2mg/mL in the keratin aqueous solution alternative embodiment 1 of isometric 2mg/mL
Solution, other steps are same as Example 1, and the self-supporting two dimension Ag films of one layer of keratin welding are formed on mixed liquor surface
(see Fig. 9), with high reflectivity.
Embodiment 9
In the present embodiment, with the lysozyme water of 2mg/mL in the stomach cardia aqueous solution alternative embodiment 1 of isometric 2mg/mL
Solution, other steps are same as Example 1, and the self-supporting two dimension Ag films of one layer of stomach cardia welding are formed on mixed liquor surface
(see Figure 10), with high reflectivity.
Embodiment 10
In the present embodiment, in the Bovine Serum Albumin in Aqueous Solution alternative embodiment 1 of isometric 2mg/mL 2mg/mL it is molten
Bacterium enzyme aqueous solution, other steps are same as Example 1, and the self-supporting of one layer of bovine serum albumin(BSA) welding is formed on mixed liquor surface
Two-dimentional Ag films (see Figure 11), with high reflectivity.
Embodiment 11
50mg lysozymes are added in 10mL ultra-pure waters, the Lysozyme in Aqueous Solution of 5mg/mL is configured to;By 40mg gold chlorides
It is added in 10mL ultra-pure waters, is configured to the aqueous solution of chloraurate of 4mg/mL;10mL ultra-pure waters are added in 40mg Sodium Citrate, usp, Dihydrate Powders
In, it is configured to the citrate dihydrate sodium water solution of 4mg/mL;By the Lysozyme in Aqueous Solution of 10mL 5mg/mL, 10mL 4mg/mL
Aqueous solution of chloraurate is uniformly mixed with the citrate dihydrate sodium water solution of 10mL 4mg/mL, and 37 DEG C stand 48 hours, in mixed liquor
Surface forms the self-supporting two dimension gold thin film of one layer of lysozyme welding (see Figure 12).Gained gold thin film is in claret, by lysozyme
Welding gold nano grain assembles.
Embodiment 12
50mg lysozymes are added in 10mL ultra-pure waters, the Lysozyme in Aqueous Solution of 5mg/mL is configured to;By five water sulphur of 250mg
Sour copper is added in 10mL ultra-pure waters, is configured to the copper sulfate solution of 25mg/mL;10mL ultra-pure waters are added in 430mg vitamin Cs
In, it is configured to the vitamin C aqueous solution of 43mg/mL;By the Lysozyme in Aqueous Solution of 10mL 5mg/mL, the sulphur of 10mL 25mg/mL
Sour copper liquor is uniformly mixed with the vitamin C aqueous solution of 10mL 43mg/mL, and 80 DEG C stand 12 hours, in mixed liquor surface shape
The self-supporting two dimension Copper thin film welded at one layer of lysozyme (see Figure 13).Gained Copper thin film is in brown, is received by lysozyme welding copper
Rice grain assembles.
Embodiment 13
50mg lysozymes are added in 10mL ultra-pure waters, the Lysozyme in Aqueous Solution of 5mg/mL is configured to;By 40mg chloroplatinic acids
It is added in 10mL ultra-pure waters, is configured to the chloroplatinic acid aqueous solution of 4mg/mL;300mg vitamin Cs are added in 10mL ultra-pure waters, are matched
The vitamin C aqueous solution of 30mg/mL is made;By the Lysozyme in Aqueous Solution of 10mL 5mg/mL, the chloroplatinic acid water of 10mL 4mg/mL
Solution is uniformly mixed with the vitamin C aqueous solution of 10mL 30mg/mL, is stored at room temperature 12 hours, and one layer is formed on mixed liquor surface
The self-supporting two dimension platinum film of lysozyme welding (see Figure 14).Gained platinum film is in grey black, and platinum nanometer is welded by lysozyme
Grain assembles.
Embodiment 14
50mg lysozymes are added in 10mL ultra-pure waters, the Lysozyme in Aqueous Solution of 5mg/mL is configured to;By 40mg gold chlorides
It is added in 10mL ultra-pure waters, is configured to the aqueous solution of chloraurate of 4mg/mL;300mg silver nitrates are added in 10mL ultra-pure waters, are matched
The silver nitrate aqueous solution of 30mg/mL is made;300mg D-Glucoses are added in 10mL ultra-pure waters, the D- of 30mg/mL is configured to
Glucose solution;By the Lysozyme in Aqueous Solution of 10mL 5mg/mL, the aqueous solution of chloraurate of 10mL 4mg/mL, 10mL 30mg/
The silver nitrate aqueous solution of mL, the D-Glucose aqueous solution of 10mL 30mg/mL are uniformly mixed, and are stored at room temperature 12 hours, in mixed liquor
Surface forms the self-supporting two-dimensional gold silver alloy film of one layer of lysozyme welding (see Figure 15).Gained electrum film is in brown green
Color is assembled by lysozyme welding gold-silver alloy nano particle.
Claims (8)
1. a kind of preparation method of self-supporting two-dimensional metallic film using protein welding, it is characterised in that:By heavy metallic salt
Solution is added in 0.02~10mg/mL protein aqueous solutions, and reducing agent, which is added, makes heavy metal ion be reduced into simple substance, i.e., molten
Liquid surface forms the self-supporting two-dimensional metallic film of one layer of protein welding.
2. the preparation method of the self-supporting two-dimensional metallic film according to claim 1 using protein welding, feature
It is:The metal salt solution is silver ammino solution, silver nitrate aqueous solution, chloroplatinic acid aqueous solution, aqueous solution of chloraurate, five water sulfuric acid
At least one of copper liquor.
3. the preparation method of the self-supporting two-dimensional metallic film according to claim 2 using protein welding, feature
It is:When the metal salt solution is silver ammino solution, by the silver ammino solution of 10~30mg/mL and 0.02~10mg/mL protein
Aqueous solution, 10~30mg/mL glucose solution be uniformly mixed in equal volume, be stored at room temperature 2~9 hours, i.e., in solution surface
Form the self-supporting two dimension Ag films of one layer of protein welding.
4. the preparation method of the self-supporting two-dimensional metallic film according to claim 2 using protein welding, feature
It is:When the metal salt solution is aqueous solution of chloraurate, by 4~5mg/mL aqueous solution of chloraurate and~10mg/mL protein
Aqueous solution, 4~5mg/mL citrate dihydrate sodium water solutions are uniformly mixed in equal volume, and 35~40 DEG C stand 24~48 hours, that is, exist
Solution surface forms the self-supporting two dimension gold thin film of one layer of protein welding.
5. the preparation method of the self-supporting two-dimensional metallic film according to claim 2 using protein welding, feature
It is:When the metal salt solution is cupric sulfate pentahydrate aqueous solution, by 20~30mg/mL cupric sulfate pentahydrates aqueous solution and 5~
10mg/mL protein aqueous solutions, 40~50mg/mL vitamin C aqueous solutions are uniformly mixed in equal volume, and 70~80 DEG C stand 10~15
Hour, i.e., the self-supporting two dimension Copper thin film of one layer of protein welding is formed in solution surface.
6. the preparation method of the self-supporting two-dimensional metallic film according to claim 2 using protein welding, feature
It is:When the metal salt solution is chloroplatinic acid aqueous solution, by 4~5mg/mL chloroplatinic acid aqueous solutions and 2~5mg/mL protein
Aqueous solution, 10~30mg/mL vitamin C aqueous solution be uniformly mixed in equal volume, be stored at room temperature 12~24 hours, i.e., in solution table
Face forms the self-supporting two dimension platinum film of one layer of protein welding.
7. the preparation method of the self-supporting two-dimensional metallic film according to claim 2 using protein welding, feature
It is:When the metal salt solution is silver nitrate aqueous solution and aqueous solution of chloraurate, by 10~30mg/mL silver nitrate aqueous solutions, 4
~5mg/mL aqueous solution of chloraurate, 2~5mg/mL protein aqueous solutions, 10~30mg/mL glucose solutions mix in equal volume
Uniformly, it is stored at room temperature 12~24 hours, i.e., the self-supporting two dimension electrum that the welding of one layer of protein is formed in solution surface is thin
Film.
8. the preparation of the self-supporting two-dimensional metallic film using protein welding according to claim 1~7 any one
Method, it is characterised in that:The protein be lysozyme, albumin, alpha-amylase, collagen, keratin, stomach cardia,
Any one in bovine serum albumin(BSA).
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CN110029331A (en) * | 2019-04-24 | 2019-07-19 | 南昌大学 | A kind of sensitizing solution and its sensitization technique for chemical plating of non-metal material copper |
CN115365494A (en) * | 2022-09-13 | 2022-11-22 | 嘉兴学院 | Preparation method of silver-coated copper powder and application of silver-coated copper powder in conductive paste |
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CN105296977A (en) * | 2015-10-29 | 2016-02-03 | 陕西师范大学 | Method for performing metal electroless deposition based on lysozyme two-dimension nano-film |
CN106835082A (en) * | 2017-01-11 | 2017-06-13 | 东南大学 | The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping |
CN107457412A (en) * | 2017-08-03 | 2017-12-12 | 吉林大学 | A kind of Jenner popped rice preparation method of high stable |
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US20040063915A1 (en) * | 2002-08-21 | 2004-04-01 | Diner Bruce A. | Metalization of microtubules |
CN104404480A (en) * | 2014-11-19 | 2015-03-11 | 无锡光旭新材料科技有限公司 | Method for preparing hydroxyapatite and bone collagen composite coating on surface of magnesium alloy |
CN105296977A (en) * | 2015-10-29 | 2016-02-03 | 陕西师范大学 | Method for performing metal electroless deposition based on lysozyme two-dimension nano-film |
CN106835082A (en) * | 2017-01-11 | 2017-06-13 | 东南大学 | The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping |
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CN110029331A (en) * | 2019-04-24 | 2019-07-19 | 南昌大学 | A kind of sensitizing solution and its sensitization technique for chemical plating of non-metal material copper |
CN115365494A (en) * | 2022-09-13 | 2022-11-22 | 嘉兴学院 | Preparation method of silver-coated copper powder and application of silver-coated copper powder in conductive paste |
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