CN106984828A - A kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching - Google Patents
A kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching Download PDFInfo
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- CN106984828A CN106984828A CN201710191161.7A CN201710191161A CN106984828A CN 106984828 A CN106984828 A CN 106984828A CN 201710191161 A CN201710191161 A CN 201710191161A CN 106984828 A CN106984828 A CN 106984828A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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
Abstract
The invention discloses a kind of fluorescence gold nanoclusters Fast back-projection algorithm new method based on chemical etching, this method comprises the following steps：Step 1: at room temperature, 10mmol/L or 50mmol/L aqueous solution of chloraurate and 10mmol/L luminol storing liquids are sufficiently mixed, deionized water or alkaline solution are added, abundant shaken well obtains mixed liquor；Step 2: adding 10mmol/L the or 50mmol/L glutathione aqueous solution in the mixed liquor that step 2 is obtained, concussion is mixed；Step 3: standing reaction, pale yellow solution is obtained, under 365nm ultraviolet source irradiation, there is obvious green fluorescence, that is, obtains gold nanoclusters solution.With ethanol solution, centrifugal purification obtains fluorescence gold nanoclusters.The preparation method is simple, quick, environmentally friendly, repeatable height.
Description
Technical field
Present invention relates particularly to a kind of gold nanoclusters Fast back-projection algorithm new method based on chemical etching, belong to fluorescence nano material
Expect preparing technical field.
Background technology
It is defined as nano-cluster with the extra small nano particle less than 2nm cluster sizes.Gold nanoclusters are by several to tens
Individual atom composition, it is closely sized to Fermi's wavelength (de Broglie wavelength of i.e. one electronics in fermi level, Jin Wei of electronics
0.5nm), its free electron has very strong quantum confined effect, ultimately results in the energy level that continuous level structure becomes discrete
Structure, shows the fluorescent characteristic of the visible near infrared region of size dependence.Compared with other fluorescent nano particles, gold nano
Cluster has longer fluorescence lifetime.Secondly as the noble metal such as gold has chemical inertness and usually contains blocking group, make its right
The toxic side effect of organism is small, with good biocompatibility and photostability.In addition, gold nanoclusters also have it is water-soluble strong,
The features such as Stokes shift is larger, makes it obtain extensive concern in terms of optics and biomedical research.
Due to fluorescence gold nanoclusters super-small, the quick high-quality gold nanoclusters of controllable preparation have certain challenge
Property.At present, the method for preparing fluorescence gold nanoclusters is broadly divided into " from bottom to top " and " from top to bottom " two class." from bottom to top "
Preparation method refers to that golden presoma is directly reduced to zeroth order gold atom, zeroth order gold in the presence of ligand molecular by appropriate reducing agent
Atom aggregation nucleating growth is nano-cluster." from top to bottom " method is the corrasion that is induced by part by gold nano grain
Size reduce, so as to obtain the gold nanoclusters of small size.The part of synthesis gold nanoclusters mainly has protein, polypeptide, amino
Acid, polymer, nucleic acid, sulfydryl small molecule etc..Although the existing method for preparing fluorescence gold nanoclusters is countless, but still
The shortcomings of so there is cumbersome preparation process, required time length, need higher reaction temperature, thus development it is a kind of it is quick, convenient,
The method that low cost prepares fluorescence gold nanoclusters has very important significance.
The content of the invention
Technical problem：Present invention aim to address the stable water-soluble gold nano cluster preparation process of current sulfydryl it is cumbersome,
The problem of time is long, proposes a kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching, to quick, convenient, low
The production water soluble fluorescence gold nanoclusters of cost.
Technical scheme：A kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching of the present invention passes through following skill
Art scheme is realized：
Step 1: at room temperature, 10mmol/L or 50mmol/L aqueous solution of chloraurate and 10mmol/L luminols are stored
Liquid is sufficiently mixed, and adds deionized water or alkaline solution, and abundant shaken well obtains mixed liquor；
Step 2: 10mmol/L the or 50mmol/L glutathione aqueous solution is added in the mixed liquor that step 2 is obtained, shake
Swing mixing；
Step 3: standing reaction, pale yellow solution is obtained, under 365nm ultraviolet source irradiation, has obvious green glimmering
Light, that is, obtain gold nanoclusters solution.
Wherein：
10mmol/L or 50mmol/L aqueous solution of chloraurate is mixed with 10mmol/L luminol storing liquids in the step one
Molar ratio be 1:1~1:4.
10mmol/L luminol storing liquids described in step one, are at room temperature, luminol to be dissolved in into 0.05mol/
It is made, is kept in dark place in Ltris-HCl buffer solutions or 0.5mol/LNaOH solution.
Described step one neutral and alkali solution is 0.05mol/Ltris-HCl buffer solutions.
Described tris-HCl buffer solutions, pH=8.5 or pH=9.0.
Process required time is stood in described step three within 2 hours.
In described step three, the temperature range for standing reaction is 18 DEG C to 90 DEG C.
Chlorauric acid solution that the addition 10mmol/L or 50mmol/L glutathione aqueous solution is added with step one rubs
Your ratio is 1:1~3:1.
Beneficial effect：The present invention is by room temperature, aqueous solution of chloraurate and luminol storing liquid being mixed, particle diameter is generated
Larger gold nano grain, adds deionized water or the fully dispersed gold nano grain of alkaline solution, then adds glutathione
The aqueous solution is performed etching to gold nano grain, and etching process can be between 18 DEG C to 90 DEG C, and etch period only needs 1-2 hours.
The preparation method of the fluorescence gold nanoclusters of the present invention can effectively prepare fluorescence gold nanoclusters, and realization quickly and conveniently obtains glimmering
Light gold nanoclusters, reduction prepares the cost and time needed for fluorescence gold nanoclusters.
Brief description of the drawings
Below, will combine drawings and Examples the invention will be further described, in accompanying drawing：
Fig. 1 is the ultraviolet spectra and fluorescence spectrum for the fluorescence gold nanoclusters that the embodiment of the present invention 17 is obtained；
Fig. 2 is the fluorescence gold nanoclusters transmission electron microscope image that the embodiment of the present invention 17 is obtained；
Fig. 3 is the grain size distribution for the fluorescence gold nanoclusters that the embodiment of the present invention 17 is obtained；
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and without
It is of the invention in limiting.As long as technical characteristic involved in the embodiments described below does not constitute conflict just each other in addition
It can be mutually combined.
Embodiment 1：Step 1: at room temperature, by 20uL 50mmol/L aqueous solution of chloraurate and 400uL 10mmol/L Shandongs
Minot/NaOH (0.5mol/L) solution is sufficiently mixed, and obtains brown suspension.Step 2: adding 40uL 50mmol/L gluathiones
The peptide aqueous solution, vibrates 2mins.1-2h is stood Step 3: being put into 90 DEG C of water-baths, pale yellow solution, i.e. gold nanoclusters are obtained molten
Liquid.
Embodiment 2：Step 1: at room temperature, by 50uL 50mmol/L aqueous solution of chloraurate and 850uL 10mmol/L Shandongs
Minot/NaOH (0.5mol/L) solution is sufficiently mixed, and obtains brown suspension.Step 2: adding 75uL 50mmol/L gluathiones
The peptide aqueous solution, vibrates 2mins.1-2h is stood Step 3: being put into 50 DEG C of water-baths, pale yellow solution, i.e. gold nanoclusters are obtained molten
Liquid.
Embodiment 3：Step 1: at room temperature, by 50uL 50mmol/L aqueous solution of chloraurate and 850uL 10mmol/L Shandongs
Minot/NaOH (0.5mol/L) solution is sufficiently mixed, and obtains brown suspension.Step 2: adding 75uL 50mmol/L gluathiones
The peptide aqueous solution, vibrates 2mins.1-2h is stood Step 3: being put into 25 DEG C of water-baths, pale yellow solution, i.e. gold nanoclusters are obtained molten
Liquid.
Embodiment 4：Step 1: at room temperature, by 50uL 50mmol/L aqueous solution of chloraurate and 850uL 10mmol/L Shandongs
Minot/NaOH (0.5mol/L) solution is sufficiently mixed, and obtains brown suspension.Step 2: adding 75uL 50mmol/L gluathiones
The peptide aqueous solution, vibrates 2mins.Step 3: standing 1-2h in the case where room temperature is 27 DEG C of environment, pale yellow solution, i.e. gold nano are obtained
Cluster solution.
Embodiment 5：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 700uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 100uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.1- is stood Step 3: being put into 90 DEG C of water-baths
2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 6：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 200uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 600uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 100uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.1- is stood Step 3: being put into 90 DEG C of water-baths
2h, obtains pale yellow solution, i.e. gold nanoclusters solution
Embodiment 7：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 600uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 200uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.1- is stood Step 3: being put into 90 DEG C of water-baths
2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 8：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 200uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 500uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 200uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.1- is stood Step 3: being put into 90 DEG C of water-baths
2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 9：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 500uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 300uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.1- is stood Step 3: being put into 90 DEG C of water-baths
2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 10：Step 1: at room temperature, by 20uL 50mmol/L aqueous solution of chloraurate and 200uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 700uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 40uL 50mmol/L glutathione aqueous solution is added, 2mins is vibrated.1-2h is stood Step 3: being put into 50 DEG C of water-baths,
Obtain pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 11：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 600uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 300uL 10mmol/L glutathione aqueous solution is added, 2mins is vibrated.Step 3: being stood in the case where room temperature is 18 DEG C of environment
1-2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 12：Step 1: at room temperature, by 100uL 10mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/NaOH (0.5mol/L) solution is sufficiently mixed, and adds 600uL deionized waters, and shaken well obtains brown suspension.Step
Rapid two, the 4uL 250mmol/L glutathione aqueous solution is added, 2mins is vibrated.Step 3: being stood in the case where room temperature is 25 DEG C of environment
1-2h, obtains pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 13：Step 1: at room temperature, by 20uL 50mmol/L aqueous solution of chloraurate and 100uL 10mmol/L
Luminol/tris (0.05mol/L, pH=8.5) solution is sufficiently mixed, and adds 800uL tris solution (0.05mol/L, pH=
8.5), shaken well obtains brown suspension.Step 2: the 300uL 10mmol/L glutathione aqueous solution is added, vibration
2mins.Step 3: standing 1-2h in the case where room temperature is 25 DEG C of environment, pale yellow solution, i.e. gold nanoclusters solution are obtained.
Embodiment 14：The present embodiment luminol/tris solution and adds tris in step one as different from Example 13
The pH=9.0 of solution.
Embodiment 15：Step 1: at room temperature, by 10uL 50mmol/L aqueous solution of chloraurate and 60uL 10mmol/L Shandongs
Minot/tris (0.05mol/L, pH=8.5) solution fully vibrates, and adds 910uL tris solution (0.05mol/L, pH=
8.5), shaken well obtains brown and mixes turbid liquid.Step 2: the 20uL 50mmol/L glutathione aqueous solution is added, vibration
2mins.Step 3: in the case where room temperature is 22 DEG C of environment, standing 1-2h, obtaining pale yellow solution, i.e. gold nanoclusters solution.
Embodiment 16：The present embodiment luminol/tris solution and adds tris in step one as different from Example 15
The volume of solution is respectively 80uL and 890uL.
Embodiment 17：The present embodiment luminol/tris solution and adds tris in step one as different from Example 15
The volume of solution is respectively 100uL and 870uL.
Fig. 1 is the uv-visible absorption spectra and fluorescence spectrum for the fluorescence gold nanoclusters that the present embodiment is obtained.Such as Fig. 1 institutes
Show, the uv-visible absorption spectra of the fluorescence gold nanoclusters of the present embodiment synthesis is not relatively large in diameter in wavelength for 520nm
The distinctive absworption peak of gold nano grain, illustrate the fluorescence gold nanoclusters that the present embodiment is obtained diameter be less than 2nm.From fluorescence light
Spectrum as can be seen that the present embodiment synthesis fluorogold nanocluster fluorescence excitation peak and emission peak position respectively be located at 420nm and
510nm。
Fig. 2 is the image that the fluorescence gold nanoclusters that the present embodiment is obtained are obtained under transmission electron microscope.Such as Fig. 2 institutes
Show, the fluorescence gold nanoclusters obtained by the present embodiment have preferable monodispersity and uniform particle diameter.
Fig. 3 is by nano-cluster diameter in the transmission electron microscope imaging to fluorescence gold nanoclusters manufactured in the present embodiment
The distribution histogram of statistics.As shown in figure 3, the diameter of the fluorescence gold nanoclusters obtained by the present embodiment be about 1.79 ±
0.4nm。
Thus upper embodiment is understood, fluorescence gold nanoclusters are prepared using method of the present invention, and step is clear simple, easy
In control, fluorescence gold nanoclusters can be effectively prepared, realization quickly and conveniently obtains fluorescence gold nanoclusters, and reduction prepares fluorescence
Cost and time needed for gold nanoclusters.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：Come for those skilled in the art
Say, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (8)
1. a kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching, it is characterised in that this method includes following step
Suddenly：
Step 1: at room temperature, 10mmol/L or 50mmol/L aqueous solution of chloraurate and 10mmol/L luminol storing liquids are filled
Divide mixing, add deionized water or alkaline solution, abundant shaken well obtains mixed liquor；
Step 2: adding 10mmol/L the or 50mmol/L glutathione aqueous solution in the mixed liquor that step 2 is obtained, concussion is mixed
It is even；
Step 3: standing reaction, pale yellow solution is obtained, under 365nm ultraviolet source irradiation, there is obvious green fluorescence,
Obtain gold nanoclusters solution.
2. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that described
10mmol/L or 50mmol/L aqueous solution of chloraurate is with the molar ratio that 10mmol/L luminol storing liquids are mixed in step one
1:1~1:4.
3. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that step
10mmol/L luminol storing liquids described in one, are at room temperature, luminol to be dissolved in into 0.05mol/Ltris-HCl bufferings
It is made, is kept in dark place in liquid or 0.5mol/LNaOH solution.
4. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that described
The step of one neutral and alkali solution be 0.05mol/Ltris-HCl buffer solutions.
5. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 4 based on chemical etching, it is characterised in that described
Tris-HCl buffer solutions, pH=8.5 or pH=9.0.
6. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that described
The step of three in stand process the time required within 2 hours.
7. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that described
The step of three in, stand reaction temperature range be 18 DEG C to 90 DEG C.
8. the fluorescence gold nanoclusters fast synthesis method as claimed in claim 1 based on chemical etching, it is characterised in that described
The mol ratio for adding the chlorauric acid solution that the 10mmol/L or 50mmol/L glutathione aqueous solution is added with step one is 1:1~3:
1。
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| CN112496336A (en) * | 2020-11-13 | 2021-03-16 | 武汉纺织大学 | Preparation method of gold nanocluster with multiple optical signal channels |
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