CN111778525A - Method for preparing chain-link gold nanowire by electrochemical method - Google Patents
Method for preparing chain-link gold nanowire by electrochemical method Download PDFInfo
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- CN111778525A CN111778525A CN202010637847.6A CN202010637847A CN111778525A CN 111778525 A CN111778525 A CN 111778525A CN 202010637847 A CN202010637847 A CN 202010637847A CN 111778525 A CN111778525 A CN 111778525A
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002848 electrochemical method Methods 0.000 title claims abstract description 13
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 23
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 20
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 19
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 19
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000006722 reduction reaction Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000010931 gold Substances 0.000 abstract description 7
- 229910052737 gold Inorganic materials 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000007795 chemical reaction product Substances 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 14
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- AQLLBJAXUCIJSR-UHFFFAOYSA-N OC(=O)C[Na] Chemical compound OC(=O)C[Na] AQLLBJAXUCIJSR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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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
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Abstract
A method for preparing chain-link gold nano-wire by electrochemical method, using polyethylene glycol, sodium carboxymethylcellulose and sodium dodecyl sulfate to form a soft template, using chloroauric acid as raw material, reducing chloroauric acid by controlling direct current voltage and the soft template at 40 ℃, washing reaction product with clear water after centrifugal separation to obtain chain-link gold nano-wire; the method directly synthesizes the chain-link gold nanowire in one step through electrochemistry, has the characteristics of simple and convenient operation and easy product separation, abandons the conventional reducing agent in gold nano-material thermochemical synthesis, is green and environment-friendly, is easy to separate, and is simple and convenient to operate.
Description
Technical Field
The invention relates to the technical field of nanoparticle preparation, in particular to a method for preparing a chain-link gold nanowire by an electrochemical method.
Background
Gold is one of the most stable elements in chemical properties, but the nano-scale gold particles have special physical and chemical properties, high electron density, dielectric property and catalytic action, and can be applied to various subjects such as medicine, food environment and the like. Because the gold nanowires have special shapes and optical properties, the gold nanowires are more and more widely applied to catalysis, photoelectronic devices and biomedicine, and particularly have great application values in the aspects of molecular markers, chemical sensing, nano electronic devices and the like. The shape of the gold nanowire synthesized at home and abroad is difficult to control at present, the principle is mainly that gold chloride is reduced by adding a chemical reducing agent, and the chemical reagents easily generate toxic action on the environment, and the traditional process flow is overall complex.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a gold nanowire with a chain-link shape by an electrochemical method, so as to solve the above disadvantages in the background art.
The technical problem solved by the invention is realized by adopting the following technical scheme:
a method for preparing a chain-link gold nanowire by an electrochemical method comprises the following steps of forming a soft template by polyethylene glycol, sodium carboxymethylcellulose and sodium dodecyl sulfate, taking chloroauric acid as a raw material, and controlling the appearance of the prepared chain-link gold nanowire by controlling direct-current voltage and the composition of the soft template under the action of a direct-current electric field, wherein the method comprises the following specific steps:
(1) preparing mixed solution
Mixing water solution containing a certain amount of polyethylene glycol, sodium carboxymethylcellulose, sodium dodecyl sulfate and chloroauric acid to form mixed solution;
(2) carrying out a reduction reaction
Placing the mixed solution obtained in the step (1) in a reaction tank, heating, and carrying out reduction reaction for 3 hours under direct current voltage;
(3) centrifugal washing
And (3) after the reduction reaction in the step (2) is finished, centrifuging the reaction solution by using a high-speed centrifuge to separate a product, and finally washing the product precipitate by using clear water to obtain the chain-link gold nanowire.
In the invention, in the step (1), the final concentration of each component in the mixed solution is as follows: 2-5 g/L of polyethylene glycol, 0.5-3 g/L of sodium carboxymethylcellulose, 2-5 g/L of sodium dodecyl sulfate and 0.2-1 mol/L of chloroauric acid.
In the invention, in the step (1), the molecular weight of the polyethylene glycol is 6000-10000, and the molecular weight of the sodium carboxymethyl cellulose is 5400-7400.
In the present invention, in the step (2), the heating temperature is 40 ℃.
In the invention, in the step (2), the direct current voltage is 1.5-20V, and the current is 0.5A.
In the invention, in the step (3), the centrifugal speed of the high-speed centrifugal machine is 8000-12000 r/min.
Has the advantages that:
(1) the invention uses polyethylene glycol (PEG), sodium carboxymethylcellulose (CMC) and sodium dodecyl sulfate to form a soft template, uses chloroauric acid as a raw material, adopts an electrochemical method to prepare the chain-shaped gold nanowire, and has the characteristics of simple and convenient operation and easy product separation, thereby effectively reducing the production cost;
(2) the direct current used in the invention is easy to obtain, the process method is simple, and the direct current can be removed by simple water washing and centrifugation after the reaction is finished, so that the final product contains less impurities and has high purity.
Drawings
FIG. 1 is a schematic diagram of spherical gold nanoparticles prepared in a preferred embodiment of the present invention.
Fig. 2 is a schematic view of a chain-link shaped gold nanowire 1 prepared in the preferred embodiment of the present invention.
Fig. 3 is a schematic view of a segmented gold nanowire 2 prepared in a preferred embodiment of the present invention.
Fig. 4 is a schematic view of a segmented gold nanowire 3 prepared in a preferred embodiment of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand and clear, the invention is further explained below by combining the specific embodiments and the drawings.
Example 1 preparation of spherical gold nanoparticles
Mixing the mixture with a certain amount of polyethylene glycol and carboxymethylSodium cellulose, sodium lauryl sulfate and chloroauric acid (HAuCl)4) The mixed solution is placed in a reaction tank, the temperature is heated to 40 ℃, the reduction reaction is carried out for 3 hours, and the final concentration of each component in the mixed solution is as follows: 3g/L of polyethylene glycol, 1.5g/L of sodium carboxymethylcellulose (CMC), 3g/L of sodium dodecyl sulfate and chloroauric acid (HAuCl)4)1mol/L；
After the reduction reaction is finished, centrifuging the reaction solution by using a high-speed centrifuge at 12000r/min to separate a product, and finally washing the product precipitate by using clear water for three times to obtain the spherical gold nanoparticles.
Example 2 preparation of chain-link gold nanowire 1
Mixing a certain amount of polyethylene glycol, sodium carboxymethylcellulose, sodium laurylsulfate and chloroauric acid (HAuCl)4) The mixed solution is placed in a reaction tank, heated to 40 ℃, and subjected to reduction reaction for 3 hours under the direct current voltage of 1.5V (0.5A), wherein the final concentration of each component in the mixed solution is as follows: 2g/L of polyethylene glycol, 0.5g/L of sodium carboxymethylcellulose (CMC), 2g/L of sodium dodecyl sulfate and chloroauric acid (HAuCl)4)0.5mol/L；
After the reduction reaction is finished, centrifuging the reaction solution by a high-speed centrifuge at 10000r/min to separate a product, and finally washing the product precipitate by clear water for three times to obtain the chain-link gold nanowire 1.
Example 3 preparation of chain-link gold nanowire 2
Mixing a certain amount of polyethylene glycol, sodium carboxymethylcellulose, sodium laurylsulfate and chloroauric acid (HAuCl)4) The mixed solution is placed in a reaction tank, heated to 40 ℃, and subjected to reduction reaction for 3 hours under the condition of direct current voltage of 10V (0.5A), wherein the final concentration of each component in the mixed solution is as follows: 2g/L of polyethylene glycol, 0.5g/L of sodium carboxymethylcellulose (CMC), 2g/L of sodium dodecyl sulfate and chloroauric acid (HAuCl)4)0.2mol/L；
After the reduction reaction is finished, centrifuging the reaction solution by a high-speed centrifuge at 10000r/min to separate a product, and finally washing the product precipitate with clear water for three times to obtain the chain-shaped gold nanowire 2.
Example 4 preparation of segmented gold nanowires 3
Mixing a certain amount of polyethylene glycol, sodium carboxymethylcellulose, sodium laurylsulfate and chloroauric acid (HAuCl)4) The mixed solution is placed in a reaction tank, heated to 40 ℃, and subjected to reduction reaction for 3 hours under the condition of direct current voltage of 20V (0.5A); the final concentration of each component in the mixed solution is as follows: 5g/L of polyethylene glycol, 3g/L of sodium carboxymethylcellulose (CMC), 5g/L of sodium dodecyl sulfate and chloroauric acid (HAuCl)4)1mol/L；
After the reduction reaction is finished, centrifuging the reaction solution by using a high-speed centrifuge for 8000r/min to separate a product, and finally washing the product precipitate for three times by using clear water to obtain the chain-shaped gold nanowire 3.
In the above examples 1 to 4, the molecular weight of polyethylene glycol was 8000 (+ -2000), and the molecular weight of sodium carboxymethylcellulose was 6400 (+ -1000); polyethylene glycol (PEG), sodium carboxymethylcellulose (CMC) and sodium dodecyl sulfate are used to form a soft template, chloroauric acid is used as a raw material, a chain-shaped gold nanowire is prepared by adopting an electrochemical method, and the gold nanowire is only different in the morphology, and the principle is as follows: the shape of the gold nanoparticles is regulated and controlled by utilizing the dual regulation and control functions of the electric field and the soft template; mixing aqueous solutions containing polyethylene glycol, sodium methylcellulose, sodium dodecyl sulfate and chloroauric acid according to a certain proportion, controlling direct current voltage and current at 40 ℃, reducing the chloroauric acid, centrifugally separating a reaction product, and washing the reaction product with clear water to obtain chain-link gold nanowires; the method can directly synthesize the chain-link gold nanowire in one step by electrochemistry, and has the characteristics of simple and convenient operation and easy product separation.
Claims (6)
1. A method for preparing a chain-link gold nanowire by an electrochemical method is characterized in that a soft template is formed by polyethylene glycol, sodium carboxymethylcellulose and sodium dodecyl sulfate, chloroauric acid is used as a raw material, and the shape of the prepared chain-link gold nanowire is regulated and controlled by controlling direct-current voltage and the soft template under the action of a direct-current electric field, and the method comprises the following specific steps:
(1) preparing mixed solution
Mixing water solution containing a certain amount of polyethylene glycol, sodium carboxymethylcellulose, sodium dodecyl sulfate and chloroauric acid to form mixed solution;
(2) carrying out a reduction reaction
Placing the mixed solution obtained in the step (1) in a reaction tank, heating, and carrying out reduction reaction for 3 hours under direct current voltage;
(3) centrifugal washing
And (3) after the reduction reaction in the step (2) is finished, centrifuging the reaction solution by using a high-speed centrifuge to separate a product, and finally washing the product precipitate by using clear water to obtain the chain-link gold nanowire.
2. The method for preparing the chain-shaped gold nanowires by the electrochemical method according to claim 1, wherein in the step (1), the final concentrations of the components in the mixed solution are as follows: 2-5 g/L of polyethylene glycol, 0.5-3 g/L of sodium carboxymethylcellulose, 2-5 g/L of sodium dodecyl sulfate and 0.2-1 mol/L of chloroauric acid.
3. The method for preparing the chain-shaped gold nanowire by the electrochemical method according to claim 1, wherein in the step (1), the molecular weight of the polyethylene glycol is 6000 to 10000, and the molecular weight of the sodium carboxymethyl cellulose is 5400 to 7400.
4. The method for electrochemically preparing the chain-shaped gold nanowires according to claim 1, wherein the heating temperature in the step (2) is 40 ℃.
5. The method for preparing the chain-shaped gold nanowires by the electrochemical method according to claim 1, wherein in the step (2), the direct current voltage is 1.5-20V, and the current is 0.5A.
6. The method for preparing the chain-shaped gold nanowires by the electrochemical method according to claim 1, wherein in the step (3), the centrifugal speed of the high-speed centrifuge is 8000-12000 r/min.
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| CN202010637847.6A CN111778525A (en) | 2020-07-06 | 2020-07-06 | Method for preparing chain-link gold nanowire by electrochemical method |
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| CN202010637847.6A CN111778525A (en) | 2020-07-06 | 2020-07-06 | Method for preparing chain-link gold nanowire by electrochemical method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015862A (en) * | 2007-03-02 | 2007-08-15 | 江南大学 | Process for preparing gold nano particle by using aqueous phase soft mould plate method |
| CN101433966A (en) * | 2008-12-17 | 2009-05-20 | 江西农业大学 | Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method |
| CN102225470A (en) * | 2011-06-20 | 2011-10-26 | 江西农业大学 | Method for preparing gold nanoparticles based on environmentally-friendly chemical method |
| CN102978666A (en) * | 2012-08-02 | 2013-03-20 | 厦门紫金矿冶技术有限公司 | Nano-gold preparation method |
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2020
- 2020-07-06 CN CN202010637847.6A patent/CN111778525A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015862A (en) * | 2007-03-02 | 2007-08-15 | 江南大学 | Process for preparing gold nano particle by using aqueous phase soft mould plate method |
| CN101433966A (en) * | 2008-12-17 | 2009-05-20 | 江西农业大学 | Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method |
| CN102225470A (en) * | 2011-06-20 | 2011-10-26 | 江西农业大学 | Method for preparing gold nanoparticles based on environmentally-friendly chemical method |
| CN102978666A (en) * | 2012-08-02 | 2013-03-20 | 厦门紫金矿冶技术有限公司 | Nano-gold preparation method |
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