CN108127124B - Preparation method of copper nanocluster with adjustable fluorescence color - Google Patents
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Abstract
The invention relates to a preparation method of a copper nanocluster with adjustable and controllable fluorescence color. According to the method, copper metal salt and quaternary ammonium salt are dissolved in deionized water, then reduction reaction is carried out, separation and purification are carried out after reaction, and the copper nanocluster with high fluorescence quantum yield is prepared. The method is simple and convenient to operate, short in time consumption, mild in reaction conditions and free of large-scale instruments, and the copper nanoclusters emitting fluorescence of different wavelengths can be obtained by adjusting the lengths of alkyl chains of different quaternary ammonium salts. The obtained copper nano-cluster has high fluorescence quantum yield, and the fluorescence emission wavelength also has the characteristic of changing along with the change of the length of the alkyl chain of the quaternary ammonium salt. The characteristics enable the copper nanocluster prepared by the method to have great potential application value in the aspects of photoelectric and luminescent device preparation, biological imaging, sensing detection and the like.
Description
Technical Field
The invention belongs to the technical field of metal nano-cluster preparation, and particularly relates to a preparation method of a copper nano-cluster with adjustable and controllable fluorescence color.
Background
Metal nanoclusters are composed of several to several hundred atoms and have optical properties similar to molecules. Compared with organic dyes and semiconductor quantum dots, the metal nanoclusters have the advantages of ultra-small particle size, low toxicity, good biocompatibility, large Stokes shift and the like. At present, a great amount of gold and silver nanoclusters are prepared for aspects such as biological imaging, sensing analysis and detection, photoelectric devices and the like. The copper nanocluster has similar luminescence property to gold and silver nanoclusters, and copper is widely distributed in nature, so that the preparation of the copper nanocluster and the research on fluorescence property are concerned.
However, the fluorescence property of copper nano-particles is still rarely applied in practice at present, and the reasons for limiting the copper nano-clusters mainly include: 1. the copper nanoclusters are small in particle size and easy to oxidize and aggregate, so that the copper nanoclusters are easy to deteriorate in the processes of preparation, purification, storage and the like; 2. a convenient and mass production preparation method is lacked; 3. the prepared copper nanocluster fails to realize the adjustability of fluorescence emission color and intensity. The fluorescence of the nanoclusters is mainly due to ligand-metal electron transfer and metal triplet radiative transitions resulting from ligand-metal electron transfer. Due to the unknown structure of the metal surface, the regulation and control of the fluorescence emission are limited.
The aggregation of the nano-clusters can adjust the acting force between ligand-metal and metal-metal, the rotation and vibration in molecules are limited through molecular aggregation, and the non-radiative transition of the molecules can be reduced, so that the radiative transition energy is increased. The nano-cluster prepared based on aggregation-induced emission fluorescence has the advantages of high fluorescence quantum yield, good stability and the like. At present, the nano-cluster aggregation induction method mainly comprises a solvent and cation induction method, however, the sizes of nano-cluster particles obtained by the two methods are not uniform. Meanwhile, the existing nano-cluster method based on induced aggregation generally adopts gold and silver nano-clusters, and the aggregation-induced preparation method of the copper nano-clusters is less.
Disclosure of Invention
The problems existing above are solved. The invention provides a preparation method of a copper nanocluster with adjustable fluorescence color. The preparation method is simple, convenient and quick, does not need harsh reaction conditions and large-scale reaction equipment, can realize batch production, and the obtained copper nano-cluster has good stability, high fluorescence quantum yield and adjustable fluorescence emission color.
The invention relates to a preparation method of a copper nanocluster with adjustable fluorescence color, which is realized by the following technical scheme:
dissolving copper ion salt and quaternary ammonium salt in water for mixed reaction, then carrying out reduction reaction by a reducing agent, separating and purifying to prepare a copper nano cluster; the method comprises the steps of reaction of copper ion salt and quaternary ammonium salt, reduction reaction, separation and purification; the method comprises the following specific steps:
(1) reacting copper ion salt with quaternary ammonium salt: dissolving copper ion salt and quaternary ammonium salt in deionized water, and mixing and stirring at the stirring speed of 600-2500 rpm. The concentration of the quaternary ammonium salt in the deionized water is 0.005-10 mol/L, and the feeding molar ratio of the copper ion salt to the quaternary ammonium salt is 0.1-8: 1;
(2) reduction reaction: and (3) stirring the mixed solution on a stirrer, dissolving a reducing agent in deionized water, and slowly adding the solution into the mixed solution to perform reduction reaction. The molar ratio of the reducing agent to the copper ion salt is 0.125-5: 1, the reaction time is 0.5-24 hours, the reaction temperature is 0-40 ℃, and the stirring speed is 600-2500 rpm.
(3) Separation and purification: centrifuging the obtained mixed solution (at a centrifugal speed of 6000 g-15300 g for 5 min-1 h), and removing the supernatant to obtain a precipitate; taking 5-10mL of deionized water to resuspend the precipitate, and then centrifuging (the centrifugal rotating speed is 6000-15300 g, and the time is 5 minutes-1 hour) to obtain the precipitate; the above washing and centrifugation were repeated three times. The resulting precipitate was dried in vacuo to give the product.
The copper ion salt is one or more than two of water-soluble copper ions, the quaternary ammonium salt is one or more than two of halogen quaternary ammonium salts containing three or four alkyl chains, and the reducing agent is one or more than two of water-soluble reducing agents.
The water-soluble copper ion salt specifically comprises the following components: copper chloride, copper bromide, copper nitrate or copper acetate.
The quaternary ammonium salt is specifically as follows: tetrapropylammonium bromide, tetrabutylammonium bromide, tetrapentylammonium bromide, tetrahexylammonium bromide, tetraheptylammonium bromide, tetraoctylammonium bromide, tetrapropylammonium chloride, tetrabutylammonium chloride, tetrapentylammonium chloride, tetrahexylammonium chloride, tetraheptylammonium chloride, tetraoctylammonium chloride, methylammonium bromide, tetramethylammonium chloride, tetraethylammonium bromide, methyltriethylammonium chloride, methyltributylammonium bromide or methyltributylammonium chloride.
The water-soluble reducing agent comprises the following components: one or more of ascorbic acid, hydrazine hydrate and sodium borohydride.
The invention has the following advantages:
1. the preparation method is simple, large-scale instruments and equipment are not needed, the cost is low, and the reaction conditions are mild;
2. the prepared copper nanocluster is high in stability and fluorescence quantum yield, and has potential application value in the aspects of biological imaging and sensing detection;
3. the fluorescent color of the copper nanocluster can be regulated and controlled by regulating the length of the alkyl chain of the quaternary ammonium salt, and the method has potential application value in the preparation of photoelectric devices;
drawings
FIG. 1 is a transmission electron micrograph of copper nanoclusters;
FIG. 2 is a transmission electron micrograph of copper nanoclusters;
FIG. 3 is a transmission electron micrograph of copper nanoclusters;
FIG. 4 is a transmission electron micrograph of copper nanoclusters;
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 method for preparing copper nanoclusters comprises the steps of dispersing copper ion salts and quaternary ammonium salts in deionized water for mixing reaction, carrying out reduction reaction by using a reducing agent, separating out solids, separating to obtain solids, and further carrying out water washing and centrifugal separation. And carrying out vacuum drying on the copper nano-cluster to obtain the copper nano-cluster.
Example 1
30 mg of tetramethylammonium bromide and 68 mg of cupric chloride dihydrate were dissolved in 8 ml of deionized water, and the mixture was stirred at a stirring speed of 750rpm for 30 minutes at a temperature of 20 ℃. 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 4 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 30 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 30 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. The solid product obtained by transmission electron microscopy analysis (see fig. 1, fig. 2) was copper nanocluster and relatively uniform in size. The obtained copper nanocluster emits yellow fluorescence under an 254nm ultraviolet lamp.
Example 2
42 mg of tetraethylammonium bromide and 68 mg of cupric chloride dihydrate were dissolved in 8 ml of deionized water, and after mixing, the mixture was stirred at a stirring speed of 750rpm for 30 minutes at a temperature of 30 ℃. Weighing 17.6 mg of ascorbic acid, dissolving 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 transferred to a 10ml centrifuge tube and centrifuged (12500g, 20 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 20 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. The solid product obtained by transmission electron microscopy analysis was copper nanoclusters (see fig. 3). The obtained copper nanocluster emits yellow fluorescence under an 254nm ultraviolet lamp.
Example 3
86 mg of tetrahexylammonium bromide and 85 mg of cupric chloride dihydrate were dissolved in 8 ml of deionized water, mixed and stirred at a stirring speed of 750rpm for 30 minutes at a 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, separating out a solid, and continuously stirring for reaction for 3 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 15 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 15 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. And further analyzing the obtained solid copper nanocluster by a transmission electron microscope.
Example 4
53 mg of tetrapropylammonium chloride and 22 mg of cupric bromide are dissolved in 8 ml of deionized water, and the mixture is stirred at the stirring speed of 2500rpm for 30 minutes at the temperature of 30 ℃. Weighing 7.6 mg of sodium borohydride, dissolving in 2 ml of deionized water, slowly dripping the sodium borohydride into the mixed solution, separating out a solid, and continuously stirring for reaction for 2 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 20 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 20 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. The solid product obtained by transmission electron microscopy analysis was copper nanoclusters (see fig. 4). The obtained copper nanocluster emits orange fluorescence under an 254nm ultraviolet lamp.
Example 5
28 mg of methyltributylammonium bromide and 36 mg of cupric acetate were dissolved in 8 ml of deionized water, mixed and stirred at 2500rpm for 30 minutes at 40 ℃. Weighing 7.6 mg of sodium borohydride, dissolving in 2 ml of deionized water, slowly dripping the sodium borohydride into the mixed solution, separating out a solid, and continuously stirring for reaction for 4 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 30 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 30 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. And further analyzing the obtained solid copper nanocluster by a transmission electron microscope. The obtained copper nanocluster emits green fluorescence under an 254nm ultraviolet lamp.
Example 6
56 mg of tetrabutylammonium chloride and 34 mg of copper chloride dihydrate were dissolved in 8 ml of deionized water, and the mixture was stirred at a stirring speed of 2000rpm for 30 minutes at a temperature of 20 ℃. 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 2 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 20 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 20 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. And further analyzing the obtained solid copper nanocluster by a transmission electron microscope. The obtained copper nanocluster emits green fluorescence under an 254nm ultraviolet lamp.
Example 7
95 mg of methyltriethylammonium bromide and 34 mg of cupric chloride dihydrate were dissolved in 10ml of deionized water, and after mixing, the mixture was stirred at a stirring speed of 2000rpm for 30 minutes at a temperature of 20 ℃. 62.5 microliter of 40% hydrazine hydrate is removed by a pipette, slowly added dropwise to the mixture to precipitate a solid, and the reaction is continued to be stirred for 2 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 20 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 20 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. And further analyzing the obtained solid copper nanocluster by a transmission electron microscope.
Example 8
78 mg of methyltributylammonium chloride and 18 mg of copper nitrate were dissolved in 8 ml of deionized water, and after mixing, stirring was carried out at a stirring speed of 2500rpm for 30 minutes at a temperature of 30 ℃. 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 transferred to a 10ml centrifuge tube and centrifuged (12500g, 30 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 30 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. The solid product obtained by further analysis by transmission electron microscopy is a copper nanocluster.
Example 9
157 mg of methyltributylammonium chloride and 22 mg of cupric bromide were dissolved in 8 ml of deionized water, mixed and stirred at 2000rpm for 30 minutes at 20 ℃. 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 2 hours. The reaction solution was transferred to a 10ml centrifuge tube and centrifuged (12500g, 30 minutes) to obtain a precipitate. And (3) washing and centrifuging the precipitate, specifically adding 10ml of deionized water to resuspend the precipitate, and centrifuging (12500g for 20 minutes) to obtain the precipitate. And (4) repeatedly washing and centrifuging for three times, and drying the precipitate in vacuum to obtain a copper nanocluster solid product. And further analyzing the obtained solid copper nanocluster by a transmission electron microscope.
Claims (5)
1. A preparation method of a copper nanocluster with adjustable fluorescence color is characterized in that the fluorescence color of the nanocluster is adjusted and controlled by adjusting the length of an alkyl chain of quaternary ammonium salt, and the preparation method comprises the steps of reacting copper ion salt with quaternary ammonium salt, reducing, separating and purifying; the method comprises the following specific steps:
(1) reacting copper ion salt with quaternary ammonium salt: dissolving copper ion salt and quaternary ammonium salt in deionized water, and mixing and stirring at the stirring speed of 600-2500 rpm; the concentration of the quaternary ammonium salt in the deionized water is 0.005-10 mol/L, and the feeding molar ratio of the copper ion salt to the quaternary ammonium salt is 0.1-8: 1;
(2) reduction reaction: stirring the mixed solution on a stirrer, dissolving a reducing agent in deionized water, and slowly adding the reducing agent into the mixed solution to perform a reduction reaction; the molar ratio of the reducing agent to the copper ion salt is 0.125-5: 1, the reaction time is 0.5-24 hours, the reaction temperature is 0-40 ℃, and the stirring speed is 600-2500 rpm;
(3) separation and purification: centrifuging the mixed solution obtained by the reaction at a centrifugal rotation speed of 6000 g-15300 g for 5 minutes-1 hour, and removing the supernatant to obtain a precipitate; taking 5-10mL of deionized water to resuspend the precipitate, and then centrifuging to obtain the precipitate; the centrifugal rotation speed is 6000-15300 g, and the time is 5 minutes-1 hour; repeating the water washing and centrifuging for three times; the resulting precipitate was dried in vacuo to give the product.
2. The method for preparing the copper nanocluster with adjustable fluorescence color according to claim 1, wherein the method comprises the following steps: the copper ion salt is one or more than two of water-soluble copper ions,
the quaternary ammonium salt is one or more than two halogen quaternary ammonium salts containing three or four alkyl chains,
the reducing agent is one or more than two of water-soluble reducing agents.
3. The method for preparing a copper nanocluster with adjustable fluorescence color according to claim 2, wherein the method comprises the following steps: the water-soluble copper ion salt is specifically as follows: copper chloride, copper bromide, copper nitrate or copper acetate.
4. The method for preparing a copper nanocluster with adjustable fluorescence color according to claim 2, wherein the method comprises the following steps: the quaternary ammonium salt is specifically tetrapropylammonium bromide, tetrabutylammonium bromide, tetrapentylammonium bromide, tetrahexylammonium bromide, tetraheptylammonium bromide, tetraoctylammonium bromide, tetrapropylammonium chloride, tetrabutylammonium chloride, tetrapentylammonium chloride, tetrahexylammonium chloride, tetraheptylammonium chloride, tetraoctylammonium chloride, methylammonium bromide, tetramethylammonium chloride, tetraethylammonium bromide, methyltriethylammonium chloride, methyltributylammonium bromide or methyltributylammonium chloride.
5. The method for preparing a copper nanocluster with adjustable fluorescence color according to claim 2, wherein the method comprises the following steps: the water-soluble reducing agent is specifically: ascorbic acid, hydrazine hydrate or sodium borohydride.
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CN108971511A (en) * | 2018-07-26 | 2018-12-11 | 大连理工大学 | A method of using polymer film as the high fluorescence copper nano-cluster of carrier rapid synthesis |
CN109128217A (en) * | 2018-11-09 | 2019-01-04 | 云南大学 | A kind of preparation method of one-step synthesis method green fluorescence copper nanocluster |
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CN110102775B (en) * | 2019-05-22 | 2022-04-29 | 西南大学 | Copper nano-cluster synthesized by taking Cu-MOFs as precursor and synthesis method |
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CN114378300B (en) * | 2022-01-21 | 2023-10-20 | 重庆科技学院 | Method for preparing nanometer copper powder by taking copper oxide as raw material |
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