CN110257897B - Preparation method of millimeter-scale one-dimensional single-crystal gold wire - Google Patents
Preparation method of millimeter-scale one-dimensional single-crystal gold wire Download PDFInfo
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000013078 crystal Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 11
- -1 halogen salt Chemical class 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000010931 gold Substances 0.000 claims description 29
- 229910052737 gold Inorganic materials 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 27
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 235000002639 sodium chloride Nutrition 0.000 claims description 20
- IWYDHOAUDWTVEP-UHFFFAOYSA-N mandelic acid Chemical compound OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 14
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- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 claims description 11
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 7
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- 238000004519 manufacturing process Methods 0.000 claims description 5
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 241000218202 Coptis Species 0.000 claims description 4
- 235000002991 Coptis groenlandica Nutrition 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000003638 chemical reducing agent Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 2
- MPOKJOWFCMDRKP-UHFFFAOYSA-N gold;hydrate Chemical compound O.[Au] MPOKJOWFCMDRKP-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 108010016626 Dipeptides Proteins 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
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- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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- 229920002258 tannic acid Polymers 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the field of micro-nano material preparation, and particularly relates to a preparation method of a millimeter-scale one-dimensional single-crystal gold wire. Under the condition of stirring, adding a solid of halogen salt into a water phase mixed solution of tetrachloroauric acid and organic molecules containing phenolic hydroxyl, dissolving and uniformly mixing, and then standing for reaction to obtain the millimeter-scale one-dimensional single-crystal gold wire. The method has the advantages of wide and easily available experimental raw materials, low requirement on experimental equipment, environmental protection and simple operation, and the obtained single crystal gold wire has millimeter-scale length, nanometer-scale diameter, high length-diameter ratio and good conductivity.
Description
Technical Field
The invention belongs to the field of preparation of low-dimensional micro-nano metal materials, and particularly relates to a preparation method of a millimeter-scale one-dimensional single-crystal gold wire.
Background
The one-dimensional micro-nano material has the advantages of high length-diameter ratio, large specific surface area, rich reactive sites and the like, and is a research hotspot in the field of materials in recent years. One-dimensional single crystal gold wires are widely used in the fields of electronics, photoelectricity, catalysis, sensing and the like due to excellent electromagnetic properties, catalytic properties, stable physicochemical properties and the like.
However, the controllable preparation of one-dimensional single-crystal gold wires, especially single-crystal gold wires having a length of the order of millimeters, is a difficult point of recent research. The search of the prior art shows that Chinese patent document No. CN 105568356A, the publication date of 2016, 5, month and 11, discloses a method for preparing gold nanowires by using a porous alumina film, the method firstly prepares a porous alumina template, and 1mol/L tetrachloroauric acid solution is deposited in the porous alumina template by an alternating current deposition (deposition voltage of 10V, frequency of 50Hz) method to obtain gold wires with the diameter of less than 100 nanometers and the length of less than 1 micrometer. The method relates to a complex template preparation process, toxic and harmful substances such as perchloric acid, phosphoric acid, chromic acid and the like are required, and the obtained gold wires are small in size and low in yield.
Also, as shown in Chinese patent document No. CN 107217280A, published in 2017, 9 and 29, a method for preparing a gold nanowire array with centimeter-sized length is disclosed, which is carried out in vacuum (less than or equal to 10)-3Pa) in an all solid state environment, with the aid of an externally applied direct current electric field (current intensity: 3-5 muA) to synthesize the gold nanometer structure (the diameter of the gold nanometer wire is distributed between 63 and 102 nm). However, although the gold wire array obtained by the method reaches centimeter level, the single crystal gold wire in the array still has nanometer scale, and the method needs high-purity gold as a material source, needs to be configured with a specific evaporation workbench, and needs to pre-deposit the fast ion conductor Rb4Cu16Cl13I7The surface of the prepared gold wire array is rough and is distributed with a large amount of gold nano particles.
In order to improve the above problems and realize green production of high-length one-dimensional single-crystal gold wires, liquid-phase chemical reduction synthesis has received attention from researchers. Single crystal gold nanowires of about 1.6nm in diameter and about 4 μm in length were synthesized at room temperature by simply mixing tetrachloroauric acid (gold source) and oleylamine (both as reducing agent and capping agent) solutions as in the literature (Nano Letters,2008,8(7): 2041-. Also, as shown in chinese patent document No. CN 109056073 a, published in 2018, 12 and 21, a method for rapidly synthesizing a hydrophilic and clean-surface single-crystal ultrafine gold-silver alloy nanowire is disclosed, in which N, N-dimethylformamide is used as a solvent, chloroauric acid, silver nitrate, a surfactant and a reducing agent are added to the system, and the mixture is stirred in an ice-water bath and heated to obtain a gold-silver alloy nanowire with a diameter of less than 2 nm. At present, because of the insufficient development of reducing agents and end capping agents, the controllability of the reduction speed and the end capping effect of a liquid phase reduction method is poor, so that the sizes of gold wires in the existing reports are limited to the nanometer level, and large-size single crystal gold wires with millimeter-level length are not found. Moreover, the preparation of one-dimensional single-crystal gold wires without strong coordination end-capping agents on the surface and with stable morphological properties still has some technical problems, such as complex preparation process, harsh reaction conditions, difficult industrial mass production and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a millimeter-scale one-dimensional single-crystal gold wire.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of millimeter-scale one-dimensional single-crystal gold thread comprises adding solid of halogen salt into the mixture of tetrachloroauric acid water solution and phenolic hydroxyl group-containing material water solution under stirring, dissolving and mixing uniformly, standing for reaction to obtain millimeter-scale one-dimensional single-crystal gold thread with length of 0.1-3 mm and diameter of 50-1000 nm; wherein,
the final concentration of the tetrachloroauric acid solid in the mixed solution is 0.1-100 mM; the mass ratio of the substance containing phenolic hydroxyl groups to the tetrachloroauric acid is 0.1-30; adding solid of halogen salt into the mixed solution, wherein the final concentration is 0.01-6M.
The tetrachloroauric acid is a gold source, the substance containing phenolic hydroxyl is a reducing agent, and the halogen salts are end capping agents.
The solid of the halogen salts is sodium chloride, potassium chloride, ammonium chloride, potassium bromide, ammonium bromide or sodium bromide; the substance containing phenolic hydroxyl groups is organic molecules with the molar mass of 94-20000g/mol and the molecular structure containing phenolic hydroxyl groups.
The substance containing phenolic hydroxyl is amino acid containing phenolic hydroxyl, dipeptide, polypeptide, hydroxyphenylacetic acid, hydroxyphenylethylamine, tannic acid, phenol and phenol compounds.
The method for preparing the millimeter-scale one-dimensional single-crystal gold wire comprises the following specific processes:
(1) tetrachloroauric acid (HAuCl) with a molar concentration of 0.1-100mM4·4H2O) the mixed solution of the aqueous solution and the aqueous solution of the substance containing the phenolic hydroxyl group is evenly mixed under the magnetic stirring of 10-6000 rpm;
(2) adding solid of halogen salt into the mixed solution under the stirring condition, and uniformly mixing; adjusting the pH value of the mixed solution to 0-7, and then standing and reacting for 6-600 hours at 50-150 ℃ under a closed condition;
(3) and (3) after the reaction is finished, collecting the precipitate to obtain a primary product, and washing the primary product by using a strong alkaline solution and deionized water in sequence to obtain the millimeter-scale one-dimensional single-crystal gold wire.
In the step (2), strong acid is adopted to adjust the pH value of the mixed solution; including but not limited to the use of hydrochloric acid, sulfuric acid, formic acid, and the like.
The washing process of the step (3) is specifically carried out in three steps: adding strong base solution with the volume 0.5-10 times of that of the reaction solution into the reaction solution, and stirring for 0.1-60 hours at the temperature of 5-90 ℃ at the stirring speed of 10-6000 rpm; secondly, transferring the solution into a suction filtration device, and filtering out alkali liquor and byproducts such as gold nanoparticles and gold nanoplates generated by reaction by using a filter membrane with the aperture of 8 microns; thirdly, washing the filter cake with a large amount of deionized water, and collecting the filter cake to obtain the gold thread.
The strong alkali solution refers to strong alkali aqueous solution with the concentration of 0.01-10M; including but not limited to aqueous solutions of strong bases such as sodium hydroxide, potassium hydroxide, and the like.
And dispersing the washed gold wire product in deionized water for storage.
The invention has the advantages of
The method has the advantages of wide and easily obtained experimental raw materials, simple preparation steps, good experimental repeatability, low requirement on experimental equipment, environmental protection and simple operation, and the obtained one-dimensional single-crystal gold wire product has millimeter-scale length, nanometer-scale diameter, high length-diameter ratio and good conductivity. The method specifically comprises the following steps:
1. the raw materials (organic molecules containing phenolic hydroxyl, halogen salts and tetrachloroauric acid) are widely and easily obtained, and the preparation process does not involve any toxic and harmful raw materials, thereby being green and environment-friendly.
2. The preparation process only needs to be carried out standing reaction in an oven or other heating devices, the requirement on experimental equipment is low, the operation is simple, and the experimental repeatability is good.
3. The invention adopts the substance containing phenolic hydroxyl as a reducing agent and the halogen salt as a capping agent to form a unique gold reduction system. The reduction capability and the end capping capability of the reaction system can be accurately controlled by changing the proportion of the reducing agent and the end capping agent, and the large-size gold single crystal is obtained.
4. The one-dimensional single-crystal gold wire product obtained by the invention has millimeter-scale length (0.1-3 mm), nanometer-scale diameter (50-1000 nm), high aspect ratio and good conductivity, has operability which is not possessed by common single-crystal nano materials, and has high yield of the single-crystal gold wire product (for example, the yield of example 1 is about 65%).
Drawings
FIG. 1 is an optical photograph of a one-dimensional single-crystal gold wire obtained in example 1 of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a one-dimensional single-crystal gold wire obtained in example 1 of the present invention.
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the end face of a one-dimensional single-crystal gold wire obtained in example 1 of the present invention.
FIG. 4 is a graph showing a contact resistance test (I-V curve) of a one-dimensional single-crystal gold wire obtained in example 1 of the present invention.
Detailed description of the preferred embodiments
The following examples illustrate the invention in detail: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
Example 1
Taking tyrosine as an example, the preparation of a millimeter-scale one-dimensional single-crystal gold wire is implemented:
tyrosine purchased from Beijing Soilebao science and technology Limited is dispersed in water (2mg/mL), and tetrachloroauric acid aqueous solution with the concentration of 10mM which is equal to the tyrosine solution is added into the tyrosine solution, and the tyrosine solution is stirred for 2 minutes to be uniformly mixed; adding sodium chloride solid to make the concentration of sodium chloride in the mixed solution be 2M; adjusting the pH of the mixed solution to 1 by using hydrochloric acid, and stirring until the mixed solution is completely dissolved. The mixture was transferred to a sealed container and allowed to stand at 80 ℃ for 5 days. Adding 20mL of 2M sodium hydroxide solution into the mixed solution, slowly stirring for 2 hours at 60 ℃, adding 50mL of deionized water, transferring the mixed solution into a suction filtration device, filtering by using a filter membrane with the aperture of 8 microns, and filtering out alkali liquor and byproducts such as gold nanoparticles and gold nanoplatelets generated by the reaction; the filter cake was washed with a large amount of deionized water, collected and stored in deionized water, to give a single-crystal gold wire product (see FIGS. 1 to 4). The yield of gold wire product was about 65%.
The morphology of the one-dimensional single crystal gold wires obtained in this example is shown in fig. 1-3, the length of the gold wires is distributed between 0.4 mm and 0.8 mm, and the average diameter is about 730 nm.
The one-dimensional single-crystal gold wire obtained above was subjected to a contact resistance test using a Gishley Keithley-4200SCS semiconductor test system (Tak, USA):
first, gold wire/water dispersion was dropped on a single crystal silicon wafer, which was ultrasonically washed with ethanol and water and blow-dried with nitrogen. And after the gold wire/water is completely dried on the silicon chip, transferring the gold wire/silicon chip to a semiconductor test system, respectively contacting probes of a semiconductor tester with two ends of the gold wire under a microscope, and testing the I-V curve of the gold wire in a voltage range of-0.55V to 0.55V.
As shown in fig. 4, gold wire has good conductivity, and combined with the operability given by its millimeter-scale length, has great potential for application as microelectrode material, electronic circuit wire, wearable electronic device accessory, and the like.
Example 2
Taking tyrosine as an example, the preparation of a millimeter-scale one-dimensional single-crystal gold wire is implemented:
the difference from the example 1 lies in:
tyrosine purchased from Beijing Soilebao science and technology Limited is dispersed in water (2mg/mL), and tetrachloroauric acid aqueous solution with the concentration of 5mM which is equal to the tyrosine solution is added into the tyrosine solution, and the tyrosine solution is stirred for 2 minutes to be uniformly mixed; adding sodium chloride solid to make the concentration of sodium chloride in the mixed solution be 3M; adjusting the pH of the mixed solution to 2 by using hydrochloric acid, and stirring until the mixed solution is completely dissolved. The mixture was transferred to a sealed container and allowed to stand at 80 ℃ for 6 days. The product was washed to obtain single-crystal gold wires having lengths distributed between 100 and 500 microns and an average diameter of about 670 nm.
The prepared gold wires have the length distribution of 0.1-0.5 mm, the average diameter of about 670 nm and the yield of about 45%.
Example 3
Taking hydroxyphenylacetic acid as an example, the preparation of a millimeter-scale one-dimensional single-crystal gold wire is implemented:
dissolving hydroxyphenylacetic acid purchased from national reagent company Limited in water to obtain hydroxyphenylacetic acid solution with the concentration of 1mg/mL, adding tetrachloroauronic acid aqueous solution with the concentration of 5mM and the volume equal to that of the hydroxyphenylacetic acid aqueous solution into the hydroxyphenylacetic acid solution, and stirring for 2 minutes to uniformly mix the mixture; adding sodium chloride solid to make the concentration of sodium chloride in the mixed solution be 2M; the pH of the mixture was adjusted to 1 with hydrochloric acid. The mixture was transferred to a sealed container and allowed to stand at 80 ℃ for 5 days. The product was washed to obtain single-crystal gold wires having lengths distributed between 0.1 and 0.5 mm.
Example 4
Taking hydroxyl phenethylamine as an example, the preparation of a millimeter-scale one-dimensional single-crystal gold wire is implemented:
dissolving hydroxyphenylethylamine purchased from national reagent company Limited in water to obtain a hydroxyphenylacetic acid solution with the concentration of 1mg/mL, adding a tetrachloroauronic acid aqueous solution with the concentration of 5mM, which has the same volume with the hydroxyphenylethylamine, and stirring for 2 minutes to uniformly mix the hydroxyphenylacetic acid solution; adding sodium chloride solid to make the concentration of sodium chloride in the mixed solution be 2M; the pH of the mixture was adjusted to 1 with hydrochloric acid. The mixture was transferred to a sealed container and allowed to stand at 80 ℃ for 5 days. The product was washed to obtain single-crystal gold wires having lengths distributed between 0.1 and 0.4 mm.
Claims (4)
1. A method for preparing a millimeter-scale one-dimensional single crystal gold wire is characterized by comprising the following steps: (1) uniformly mixing a mixed solution of a tetrachloroauric acid aqueous solution with a molar concentration of 0.1-100mM and an aqueous solution of a substance containing phenolic hydroxyl under magnetic stirring at 10-6000 rpm;
(2) adding solid of halogen salt into the mixed solution under the stirring condition, and uniformly mixing; adjusting the pH of the mixed solution to be 0-7, and then standing and reacting for 6-600 hours at 50-150 ℃ under a closed condition;
(3) after the reaction is finished, collecting the precipitate to obtain a primary product, and washing the primary product by using a strong alkaline solution and deionized water in sequence to obtain a single crystal gold wire with the millimeter scale and the one-dimensional length of 0.1-3 mm and the diameter of 50-1000 nm;
wherein the mass ratio of the substance containing phenolic hydroxyl groups to the tetrachloroauric acid is 0.1-30; the final concentration of the solid of the halogen salts in the mixed solution is 0.01-6M;
the washing process of the step (3) is specifically carried out in three steps: adding strong base solution with the volume 0.5-10 times of that of the reaction solution into the reaction solution, and stirring for 0.1-60 hours at the temperature of 5-90 ℃ at the stirring speed of 10-6000 rpm; secondly, transferring the solution into a suction filtration device, and filtering alkali liquor and gold nano-particles and gold nano-sheet byproducts generated by reaction by using a filter membrane with the aperture of 8 microns; thirdly, washing the filter cake with a large amount of deionized water, and collecting the filter cake to obtain the gold thread;
the solid of the halogen salts is sodium chloride, potassium chloride, ammonium chloride, potassium bromide, ammonium bromide or sodium bromide; the substance containing phenolic hydroxyl is hydroxyphenylacetic acid, hydroxyphenylethylamine or tyrosine.
2. A method for producing a single-dimensional single-crystal gold wire of millimeter size according to claim 1, characterized in that: and (3) adjusting the pH value of the mixed solution by using strong acid in the step (2).
3. A method for producing a single-dimensional single-crystal gold wire of millimeter size according to claim 1, characterized in that: the strong alkali solution refers to a strong alkali water solution with the concentration of 0.01-10M.
4. A method for producing a single-dimensional single-crystal gold wire of millimeter size according to claim 1, characterized in that: and dispersing the washed gold wire product in deionized water for storage.
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