CN108127125B - Preparation method of high-stability copper nanosheet - Google Patents
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- CN108127125B CN108127125B CN201611091728.5A CN201611091728A CN108127125B CN 108127125 B CN108127125 B CN 108127125B CN 201611091728 A CN201611091728 A CN 201611091728A CN 108127125 B CN108127125 B CN 108127125B
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Abstract
The invention provides a preparation method of a high-stability copper nanosheet. The method is simple and convenient to operate, short in time consumption, large-scale instruments and harsh reaction conditions are not needed, and the copper nanosheets with different fluorescence emission intensities can be obtained by adjusting the proportion of the alkyl trimethyl quaternary ammonium salt, the copper ion salt and the reducing agent. The copper nanosheet obtained by the method is good in stability and high in fluorescence efficiency, and has potential application values in the aspects of photoelectric device preparation, sensing detection and the like.
Description
Technical Field
The invention belongs to the field of metal nano materials, and particularly relates to a preparation method of a high-stability copper nanosheet.
Background
By metallic nanomaterials in the broad sense is meant that at least one dimension of the three-dimensional system is in the nanometer size range (1-100nm) or is made up of these elementary units. The nano material has the advantages of high catalytic activity, high light absorption capacity, good plasticity, high hardness, high conductivity, high diffusivity, high specific heat and the like, so that the nano material has great application value in optical, electrical, catalytic and magnetic nano materials.
Because copper is abundant in natural resources and the copper nano material has excellent performances similar to those of gold and silver nano materials in the aspects of optics, electrics and the like, the copper nano material attracts wide attention in the last two decades. Compared with gold and silver nanometer materials, although copper is abundant in natural resources and cheaper in price, the stability is poor. At present, many methods for synthesizing copper nano-materials exist, including hydrothermal synthesis, gas evaporation, sol-gel method, laser ablation, electrochemical method, etc. Among them, the synthesis of copper nanomaterials using water-soluble high molecular organic substances or surfactants as ligands has attracted much attention because of the reduction of environmental pollution without using organic solvents. However, the copper nano material obtained by the methods is easy to oxidize and has the defect of poor stability, and the synthesized copper nano material can not be stored for a long time under the protection of inert gas.
Disclosure of Invention
The problems existing above are solved. The invention provides a preparation method of a high-stability copper nanosheet. The preparation method is convenient and fast, the reaction condition is mild, large-scale instruments are not needed, batch production can be realized, and the prepared copper nanosheet is good in stability and adjustable in fluorescence emission intensity.
The invention relates to a preparation method of a high-stability copper nanosheet.
The method comprises the steps of reaction of copper ion salt and alkyl trimethyl quaternary ammonium salt type surfactant, reduction reaction, separation and purification; the method comprises the following specific steps:
(1) copper ion salt reacts with alkyl trimethyl quaternary ammonium salt type surfactant: weighing a copper ion salt and an alkyl trimethyl quaternary ammonium salt surfactant in a reaction container, adding deionized water, stirring for dissolving, wherein the stirring time is 1-5 hours, and the stirring speed is 500-2500 rpm. The concentration of the alkyl trimethyl quaternary ammonium salt surfactant in deionized water is 0.005-5 mol/L, and the feeding molar ratio of the copper ion salt to the alkyl trimethyl quaternary ammonium salt surfactant is 0.05-10: 1;
(2) reduction reaction: dissolving a reducing agent in deionized water, slowly and dropwise adding the solution in the step (1), and stirring for reaction. The reaction time is 0.5 to 24 hours, and the stirring speed is 500 to 2000 rpm. The molar ratio of the reducing agent to the copper ion salt is 0.05-5: 1.
(3) Separation and purification: (2) the obtained mixed solution is centrifugally separated to obtain sediment. The washing and the centrifugation are repeated for three times, 5-10 ml of water is added for each time for heavy suspension, and the supernatant is discarded after the centrifugation. The centrifugal rotation speed is 6000-15000 g, and the time is 0.1-1 hour. And drying the obtained product in vacuum to obtain the copper nanosheet.
The alkyl trimethyl quaternary ammonium salt surfactant is one or more than two halogen quaternary ammonium salts which can be dissolved in water and contain three methyl groups and one alkyl long chain, the copper ion salt is one or more than two water-soluble divalent copper ion salts, and the reducing agent is one or more than two water-soluble reducing agents.
The alkyl trimethyl quaternary ammonium salt surfactant specifically comprises: octadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride, heptadecyl trimethyl ammonium bromide, heptadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, and/or dodecyl trimethyl ammonium chloride.
The water-soluble copper ion salt specifically comprises the following components: one or more of copper chloride, copper bromide, copper nitrate and copper acetate.
The water-soluble reducing agent comprises: one or more of ascorbic acid, hydrazine hydrate and sodium borohydride.
The invention has the following advantages:
1. large-scale instruments and equipment are not needed, the preparation cost is low, the method is simple and convenient, and the reaction conditions are mild;
2. the prepared copper nanosheet is high in stability and has potential application value in the preparation of materials such as optics, electricity and catalysis;
3. the fluorescence intensity of the copper nanosheets can be regulated and controlled by adjusting the proportion of the copper ion salt, the alkyl trimethyl quaternary ammonium salt surfactant and the reducing agent, and the copper nanosheets have potential application values in the fields of biological imaging, sensing detection and the like;
drawings
FIG. 1, transmission electron micrograph of copper nanoplates;
FIG. 2 is a transmission electron micrograph of copper nanoplates;
FIG. 3 is a scanning electron micrograph of copper nanoplates.
Detailed description of the invention
The present invention is described in further detail below with reference to examples, but it should not be construed that the present invention is limited to the examples, and any technologies implemented based on the present invention should be considered as the scope of the present invention.
A preparation method of copper nanosheets comprises the steps of dispersing a copper ion salt and an alkyl trimethyl quaternary ammonium salt surfactant in deionized water for mixing reaction, adding a reducing agent for reduction, separating to obtain a solid, further washing with water for purification, and drying in vacuum to obtain the copper nanosheets.
Example 1
36 mg of hexadecyl trimethyl ammonium bromide and 68 mg of copper chloride dihydrate are weighed into a reaction vessel, 8 ml of deionized water is added, stirring is carried out for dissolution, the stirring speed is 1700rpm, and stirring is carried out for 30 minutes, and the temperature is 25 ℃. 3.8 mg of sodium borohydride is weighed and dissolved in 2 ml of deionized water, the mixture is slowly dripped into the mixture, solid is separated out, and the reaction is continuously stirred for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. Analysis by scanning electron microscopy (see fig. 3) and transmission electron microscopy (see fig. 1, 2) revealed that the resulting solid product was copper nanoplates. The obtained copper nanosheet emits yellow fluorescence under an ultraviolet lamp with the wavelength of 254 nm.
Example 2
Weighing 360 mg of hexadecyl trimethyl ammonium bromide and 112 mg of copper bromide into a reaction container, adding 8 ml of deionized water, stirring and dissolving, wherein the stirring speed is 1700rpm, and the stirring time is 30 minutes, and the temperature is 25 ℃. 3.8 mg of sodium borohydride is weighed and dissolved in 2 ml of deionized water, the mixture is slowly dripped into the mixture, solid is separated out, and the reaction is continuously stirred for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope. The obtained copper nanosheet emits orange fluorescence under an ultraviolet lamp with the wavelength of 254 nm.
Example 3
Weighing 32 mg of dodecyl ammonium chloride and 34 mg of copper chloride dihydrate into a reaction vessel, adding 8 ml of deionized water, stirring for dissolving, wherein the stirring speed is 1000rpm, and stirring is carried out for 30 minutes at the temperature of 25 ℃. Weighing 7.6 mg of sodium borohydride, dissolving in 2 ml of deionized water, slowly dripping the sodium borohydride into the mixed solution to separate out a solid, and continuously stirring for reaction for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. The pellet was resuspended in 10ml of deionized water and centrifuged (12500g, 10 minutes) to obtain a pellet. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope. The obtained copper nanosheet emits orange fluorescence under an ultraviolet lamp with the wavelength of 254 nm.
Example 4
Weighing 33 mg of tetradecyltrimethylammonium bromide and 68 mg of cupric chloride dihydrate into a reaction vessel, adding 8 ml of deionized water, stirring for dissolution at the stirring speed of 1700rpm for 30 minutes at the temperature of 25 ℃. Weighing 17 mg of ascorbic acid, dissolving the ascorbic acid in 2 ml of deionized water, slowly dripping the ascorbic acid into the mixed solution to separate out a solid, and continuously stirring for reaction for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. The pellet was resuspended in 10ml of deionized water and centrifuged (12500g, 10 minutes) to obtain a pellet. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope.
Example 5
39 mg of octadecyl trimethyl ammonium bromide and 68 mg of copper chloride dihydrate are weighed into a reaction vessel, 8 ml of deionized water is added, the mixture is stirred and dissolved, the stirring speed is 1700rpm, the stirring time is 30 minutes, and the temperature is 40 ℃. 3.8 mg of sodium borohydride is weighed and dissolved in 2 ml of deionized water, the mixture is slowly dripped into the mixture, solid is separated out, and the reaction is continuously stirred for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope. The obtained copper nanosheet emits yellow fluorescence under an ultraviolet lamp with the wavelength of 254 nm.
Example 6
34 mg of tetradecyltrimethylammonium bromide and 37 mg of cupric nitrate are weighed into a reaction vessel, 8 ml of deionized water is added, stirring is carried out for dissolution, the stirring speed is 1700rpm, the stirring is carried out for 30 minutes, and the temperature is 40 ℃. 3.8 mg of sodium borohydride is weighed and dissolved in 2 ml of deionized water, the mixture is slowly dripped into the mixture, solid is separated out, and the reaction is continuously stirred for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope.
Example 7
47 mg of decaalkyltrimethylammonium chloride and 36 mg of copper acetate are weighed into a reaction vessel, 8 ml of deionized water is added, stirring is carried out at the speed of 1700rpm for 30 minutes while stirring is carried out, and the temperature is 25 ℃. 3.8 mg of sodium borohydride is weighed and dissolved in 2 ml of deionized water, the mixture is slowly dripped into the mixture, solid is separated out, and the reaction is continuously stirred for 1 hour. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope.
Example 8
Weighing 67 mg of tetradecyltrimethylammonium bromide and 85 mg of cupric chloride dihydrate into a reaction vessel, adding 10ml of deionized water, stirring for dissolving, wherein the stirring speed is 1700rpm, and stirring is carried out for 30 minutes at the temperature of 25 ℃. 62.5 microliter of 40% hydrazine hydrate is removed by pipetting and slowly added dropwise to the mixture to precipitate a solid, and the reaction is continued for 1 hour with stirring. The reaction solution was centrifuged (12500g, 30 minutes) to obtain a precipitate. 10ml of deionized water was added to resuspend the pellet, and the pellet was centrifuged (12500g, 10 minutes) and the supernatant discarded. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanosheet solid product. And further analyzing the obtained copper nanosheet through a scanning electron microscope and a transmission electron microscope.
Claims (5)
1. A preparation method of a high-stability fluorescent copper nanosheet is characterized by comprising the steps of reacting a copper ion salt with an alkyl trimethyl quaternary ammonium salt type surfactant, reducing, separating and purifying; the fluorescence intensity of the copper nanosheet can be regulated and controlled by adjusting the proportion of the copper ion salt, the alkyl trimethyl quaternary ammonium salt surfactant and the reducing agent, and the method comprises the following specific steps:
(1) copper ion salt reacts with alkyl trimethyl quaternary ammonium salt type surfactant: weighing a copper ion salt and an alkyl trimethyl quaternary ammonium salt surfactant in a container, adding deionized water, stirring for dissolving, wherein the stirring time is 1-5 hours, and the stirring speed is 500-2500 rpm; the concentration of the alkyl trimethyl quaternary ammonium salt surfactant in deionized water is 0.005-5 mol/L, and the feeding molar ratio of the copper ion salt to the alkyl trimethyl quaternary ammonium salt surfactant is 0.05-10: 1;
(2) reduction reaction: dissolving a reducing agent in deionized water, slowly dripping the solution obtained in the step (1), and stirring for reaction; the reaction time is 0.5-24 hours, the reaction temperature is 25 ℃, and the stirring speed is 500-2500 rpm; the molar ratio of the reducing agent to the copper ion salt is 0.05-5: 1;
(3) separation and purification: centrifuging the mixed solution obtained in the step (2) to obtain a precipitate; washing and centrifuging for three times, adding 5-10 ml of water for resuspension each time, centrifuging and discarding the supernatant; the centrifugal rotation speed is 6000-15000 g, and the time is 0.1-1 hour; and drying the obtained product in vacuum to obtain the copper nanosheet.
2. The preparation method of the high-stability fluorescent copper nanosheet according to claim 1, wherein: the alkyl trimethyl quaternary ammonium salt surfactant is one or more than two halogen quaternary ammonium salts which can be dissolved in water and contain three methyl groups and one alkyl long chain, the copper ion salt is one or more than two water-soluble divalent copper ion salts, and the reducing agent is one or more than two water-soluble reducing agents.
3. The preparation method of the high-stability fluorescent copper nanosheet according to claim 2, wherein: the alkyl trimethyl quaternary ammonium salt surfactant specifically comprises: octadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride, heptadecyl trimethyl ammonium bromide, heptadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide or dodecyl trimethyl ammonium chloride.
4. The preparation method of the high-stability fluorescent copper nanosheet according to claim 2, wherein the water-soluble copper ion salt is specifically: one or more of copper chloride, copper bromide, copper nitrate or copper acetate.
5. The method for preparing a high-stability fluorescent copper nanosheet according to claim 2, wherein the water-soluble reducing agent is one or more than two of ascorbic acid, hydrazine hydrate and sodium borohydride.
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| US11131031B2 (en) * | 2018-06-12 | 2021-09-28 | Honda Motor Co., Ltd. | High-yield preparation of two-dimensional copper nanosheets |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN113059173B (en) * | 2021-03-23 | 2022-02-08 | 西北有色金属研究院 | Preparation method of foliated porous copper nanosheet |
| CN114346254B (en) * | 2022-01-21 | 2023-08-18 | 重庆科技学院 | Method for preparing nanometer copper powder in eutectic ionic liquid |
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| CN101890504A (en) * | 2010-07-07 | 2010-11-24 | 江苏技术师范学院 | Preparation method of flaky nano copper powder |
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