CN115283688B - Method for preparing gold nanoclusters by using solid-phase kinetic control method - Google Patents
Method for preparing gold nanoclusters by using solid-phase kinetic control method Download PDFInfo
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- CN115283688B CN115283688B CN202210781637.3A CN202210781637A CN115283688B CN 115283688 B CN115283688 B CN 115283688B CN 202210781637 A CN202210781637 A CN 202210781637A CN 115283688 B CN115283688 B CN 115283688B
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- sodium cyanoborohydride
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- 239000010931 gold Substances 0.000 title claims abstract description 53
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007790 solid phase Substances 0.000 title claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- BEOOHQFXGBMRKU-UHFFFAOYSA-N sodium cyanoborohydride Chemical compound [Na+].[B-]C#N BEOOHQFXGBMRKU-UHFFFAOYSA-N 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 10
- 108010024636 Glutathione Proteins 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 238000009777 vacuum freeze-drying Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
- 230000033228 biological regulation Effects 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 229960003180 glutathione Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000002431 foraging effect Effects 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- XYYVDQWGDNRQDA-UHFFFAOYSA-K trichlorogold;trihydrate;hydrochloride Chemical compound O.O.O.Cl.Cl[Au](Cl)Cl XYYVDQWGDNRQDA-UHFFFAOYSA-K 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
Classifications
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
Abstract
The invention discloses a method for regulating and controlling gold nanocluster growth by using solid phase dynamics, belonging to the field of nanomaterial synthesis. The invention adopts a mild kinetic regulation means to prepare the gold nanocluster with a specific scale. Different sizes of nanoclusters can be prepared by utilizing a dynamic regulation method, so that the formation process of the nanoclusters is better known. Compared with the existing nano material cluster synthesis method, the method provided by the invention has the advantages of simplicity in regulation and control, strong operability and universal applicability. The method can not only provide a synthesis method for regulating and controlling the gold nanocluster, but also can apply the prepared gold nanocluster to the fields of catalysis, sensing, medical treatment and the like. The invention aims to provide a method for regulating and controlling the growth of gold nanoclusters, so as to prepare gold nanoclusters with different scales. The method has simple dynamic regulation and control process, is easy to realize the preparation of gold nanoclusters with different scales, and has wide synthesis applicability for regulating and controlling the nanoclusters such as copper, silver and the like.
Description
Technical Field
The invention belongs to the field of nanocluster synthesis, and in particular relates to a novel gold nanocluster prepared by adopting tetrachloroauric acid trihydrate and L-reduced glutathione as precursors and through the kinetic control action and the coordination action between gold and glutathione.
Background
Noble metal nanoparticles (e.g., gold, silver) have become one of the most important nanomaterial types widely explored in nanoscience and nanotechnology research. There are two different size ranges of particular interest between metal atoms and bulk metals, namely the cluster state and the nanocrystalline state. Metal nanoclusters, which are typically sized from sub-nanometers to about 2nm (core diameter). Due to the strong quantum confinement of electrons in this very small size range, electron energy quantization occurs, which effect greatly alters the physical and chemical properties of the metal clusters, e.g. plasma excitation of metal nanocrystals no longer exists in the cluster state. Small metal clusters behave like molecules, exhibiting stronger catalytic activity, luminescence, and unique optoelectronic properties, which makes this type of nanomaterial very promising in the development of new generation catalysts, sensors, and optoelectronic devices.
Although having significant success in gold cluster synthesis, most synthesis processes are affected by producing mixtures of clusters of different sizes, and typically the yield of a particular size is quite low; therefore, the product must be separated on the basis of techniques such as separation crystallization, chromatography, electrophoresis, etc. The difficulty in purification of the clusters has been a major obstacle to practical use of the cluster materials. It is therefore particularly necessary to regulate nanocluster growth. It is believed that by carefully controlling the reaction kinetics of the cluster synthesis reaction, it should be possible to create a specific chemical environment that results in the formation of clusters of one size and the inhibition of clusters of other sizes. In this respect, we propose to synthesize gold nanoclusters by kinetic modulation, a potential method that can modulate gold nanoclusters of different scales.
Disclosure of Invention
[ problem to be solved ]
The invention aims to provide a method for dynamically regulating and controlling the growth of gold nanoclusters, so as to prepare gold nanoclusters with different scales. The synthesis method is simple, the synthesis condition is mild, the dynamics regulation and control process is simple, the preparation of gold nanoclusters with different scales is easy to realize, and the applicability to synthesizing nanoclusters of copper, silver and the like is wide.
Technical scheme
The invention adopts the following technical scheme:
the invention utilizes HAuCl 4 ·3H 2 The coordination effect of O and L-reduced glutathione is that the precursor is grinded to form Au (I) -SR precursor. And then adding a mild reducing agent sodium cyanoborohydride into an agate mortar for dynamic regulation, and adding a small amount of water after the sodium cyanoborohydride is sufficiently ground to ensure that the sodium cyanoborohydride is sufficiently ground, wherein the Au (I) is further reduced into the Au (0) under the action of the reducing agent to form the inner core of the gold nanocluster. And then standing the mixture at room temperature for a period of time, then placing the mixture into a refrigerator for aging, and centrifuging, washing and vacuum drying the obtained solution to obtain the gold nanocluster. The invention provides a method for preparing gold nanoclusters by using a kinetic means, which can regulate and control the synthesis of gold nanoclusters with specific dimensions.
The present invention will be described in detail below.
A method for preparing gold nanoclusters by a solid phase kinetic control method, comprising the following steps:
A. preparation of Au (I) -SR precursor
Weighing a certain amount of HAuCl 4 ·3H 2 O and L-reduced glutathione (L-GSH) are placed in an agate mortar, and the precursors are fully ground, so that a pale yellow Au (I) -SR precursor is obtained.
In the present invention, due to HAuCl 4 ·3H 2 The coordination of O and L-GSH is fully grinded to form an Au (I) -SR precursor which is an intermediate product in the cluster synthesis process, and the preparation of the Au (I) -SR precursor can influence the final yield of clusters.
B. Reduction of Au (I) -SR precursors
Weighing a certain amount of sodium cyanoborohydride, adding the sodium cyanoborohydride into an agate mortar in the A, and grinding the sodium cyanoborohydride for a certain time, wherein the sodium cyanoborohydride is difficult to grind due to water absorption, and a small amount of water is needed to grind Au (I) -SR and sodium cyanoborohydride more fully; then adding a certain amount of water, slowly stirring by using a grinding rod, collecting the solution, standing at room temperature for a period of time, and then aging in a refrigerator.
According to the invention, the Au (I) -SR precursor slowly grows under the action of sodium cyanoborohydride, and the Au nanoclusters can be ground more fully after a small amount of water is added; the effect of standing for a period of time at room temperature is to accelerate the growth of gold nanoclusters, and the effect of standing in a refrigerator is to slow down the growth of gold nanoclusters, so that the growth of gold nanoclusters with different scales can be regulated and controlled, and the specific gold nanoclusters are obtained.
C. Preparation of gold nanoclusters
And (3) adding 15mL of methanol into the liquid in the step (B) to perform precipitation, centrifugation, washing and vacuum drying to obtain a product.
In the invention, after methanol is added, gold nanoclusters quickly settle down, so that the gold nanoclusters can be obtained through centrifugation, washing and drying.
The gold nanocluster prepared by the dynamic means can obtain a peak of 720nm under an ultraviolet spectrum test and a peak of 780nm under a fluorescence spectrophotometer test, which shows that the gold nanocluster has unique optical properties and can be applied to the fields of photoelectricity, catalysis, sensing, catalysis and the like.
[ advantageous effects ]
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art, the gold nanocluster prepared by the method has the advantages of simple process, mild dynamic regulation and control means and easy operation, and can obtain nanoclusters with specific dimensions; can be popularized to the synthesis of nanoclusters such as copper, silver and the like. The usage amount of the reducing agent, the aging time and the aging temperature are regulated, so that the nanocluster with a specific scale is prepared; the raw materials of the prepared clusters are easy to obtain, and the preparation process is high; the prepared cluster shows unique physical and chemical properties.
Drawings
FIG. 1 is a transmission electron microscope image of gold nanoclusters prepared by the method;
FIG. 2 ultraviolet visible spectrum of gold nanoclusters
Detailed Description
The invention is further illustrated and described below in connection with the following examples of the invention.
Weigh 62mg of HAuCl 4 ·3H 2 Placing O and 234mg of L-reduced glutathione into an agate mortar, and obtaining a pale yellow sample after the O and the 234mg of L-reduced glutathione are sufficiently ground; then, 76mg of sodium cyanoborohydride was weighed and added thereto, and was ground with an agate mortar rod, and grinding of sodium cyanoborohydride was made difficult due to its water absorption, and 100uL of water was added at this time, so that Au (I) -SR and sodium cyanoborohydride were ground more sufficiently; then 10mL of water was added and slowly stirred with a mortar bar, the solution was collected and left to stand at room temperature for 30minutes, then placed in a refrigerator for aging for 1 hour.
Claims (1)
1. A method for preparing gold nanoclusters by a solid phase kinetic control method, which is characterized by comprising the following steps:
A. preparation of Au (I) -SR precursor
Weighing a certain amount of HAuCl 4 ·3H 2 Placing O and L-reduced glutathione in an agate mortar, fully grinding the O and L-reduced glutathione by an agate mortar rod for 20min, and changing the color from white to light yellow in the grinding process to finally obtain a light yellow Au (I) -SR precursor;
B. reduction of Au (I) -SR precursors
Weighing a certain amount of sodium cyanoborohydride, adding the sodium cyanoborohydride into an agate mortar in the A, grinding the sodium cyanoborohydride by an agate mortar rod for a period of time, adding a small amount of water, and grinding for 5 minutes, wherein the solution turns light black; adding a certain amount of water, rapidly stirring with an agate mortar rod, standing at room temperature for 30min, and aging in a refrigerator at 3 ℃ for 1h after the target product is formed;
C. preparation of gold nanoclusters
B, precipitating, centrifuging, washing, vacuum drying or freeze drying the liquid in the step B to obtain clusters;
in step A, the HAuCl 4 ·3H 2 O, L-reduced glutathione has the mass of 62mg and 234mg respectively;
in step B, the mass of sodium cyanoborohydride is 76mg; the temperature of the small amount of water added for the first time is 25 ℃, and the volume is 100 mu L; the temperature of a certain amount of water added for the second time is 25 ℃, and the volume is 10mL;
in step C, the selected centrifugal speed is 9000rpm; the solvent selected was methanol, 15mL in volume, washed to give pure clusters and the unreacted chloroauric acid and Au (I) -SR precursor were removed; the number of times of washing was 3 times; the time for vacuum drying was 30min.
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| CN202210781637.3A CN115283688B (en) | 2022-07-04 | 2022-07-04 | Method for preparing gold nanoclusters by using solid-phase kinetic control method |
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| CN116656344B (en) * | 2023-05-12 | 2024-04-12 | 电子科技大学 | Preparation method of fluorescent nanocluster for humidity sensor |
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