CN104014813B - A kind of preparation method of the nano-Au solution based on Ago-Gel - Google Patents
A kind of preparation method of the nano-Au solution based on Ago-Gel Download PDFInfo
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Abstract
The preparation method who the invention discloses a kind of nano-Au solution based on Ago-Gel, comprises the following steps: (1) adds Ago-Gel in water, heats to obtain the uniform agarose solution of clarification; (2) in agarose solution, add chlorauric acid solution, constant temperature stirs, and mixed solution normal temperature is placed, and obtains nm of gold gel; (3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, obtains nano-Au solution after washing. Described nano-Au solution is dispersed in water and is formed by nanogold particle, described nanogold particle size uniform, and average grain diameter is 1～10nm. The present invention relates to that preparation is simple, the reducing agent of use is Ago-Gel, common nontoxic, and the nanogold particle size uniform making is controlled, and particle diameter is little, and is difficult for reuniting. This method has important actual application value in the preparation field of nm of gold.
Description
Technical field
The present invention relates to a kind of preparation method of the nano-Au solution based on Ago-Gel.
Background technology
Nm of gold, owing to possessing many special natures such as quantum size effect, macro quanta tunnel effect and skin effect, extensively shouldFor electrochemical probe, optical probe, DNA detection, biochemical analysis, catalyst, colloidal sol, plant protection and Raman scattering etc.Field.
Small size nm of gold has higher specific area and larger charge density, and catalytic activity is higher, actual application prospectLarger than large-sized nm of gold. At present, the condition harshness of synthetic small size nm of gold, complex steps, agents useful for same is more. YellowMoral vigorously waits [CN1663714A] taking hydrazine hydrate as reducing agent, and taking polyvinylpyrrolidone and lauryl sodium sulfate as additive systemThe standby nano-Au solution that obtains; Dong Shouan etc. [CN1554503A] are taking acetone as reducing agent and add the protective agents such as polyvinyl alcohol and be prepared intoTo nano Au particle. In the preparation method of report, except reducing agent, often need to introduce other additive at present, as dispersant, stableAgent, protective agent or flocculant etc., and may use larger, the with serious pollution organic solvent of toxicity, be unfavorable for carrying out extensive use.
Therefore, further find technique simple, the preparation method of raw materials used common nontoxic small size nm of gold, has importantPractical significance.
Summary of the invention
The object of the invention is to, provide a kind of technique simple, raw materials used environment amenable nm of gold preparation method, adoptsThe nanogold particle size that described method makes is controlled, and particle diameter is very little, and is difficult for reuniting.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for nano-Au solution based on Ago-Gel, comprises the following steps:
(1) in water, add Ago-Gel, be placed in water bath and heat, must clarify uniform agarose solution;
(2) in agarose solution, add chlorauric acid solution, constant temperature stirs, in this process, and the hydroxyl that agarose is rich inGold ion in gold chloride is reduced into gold particle, mixed solution normal temperature is placed, gold particle is embedded in the agarose forming graduallyIn the internal cavities of gel, obtain nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, washs to obtain described nano-Au solution.
Water in described step (1) is ultra-pure water.
In described agarose solution, add after chlorauric acid solution, the concentration of agarose in the mixed solution obtaining is0.08～0.15g/mL. The concentration of described chlorauric acid solution is 0.02～2.5mM.
Described agarose solution and chlorauric acid solution volume ratio are (1～9): 1.
Described constant temperature whipping temp is 80～100 DEG C, and constant temperature mixing time is 3～5min, and normal temperature temperature is 20～30 DEG C, and normal temperature is putThe time of putting is 1～15d.
Described washing step is with ultra-pure water washing 3 times.
Described nano-Au solution is dispersed in water and is formed by nanogold particle, nanogold particle size uniform, and particle diameter is very little,Average grain diameter is 1～10nm.
The size of nanogold particle is controlled, realizes with the internal cavities size of controlling gel by the concentration that regulates agarose.
Compared with prior art, the invention has the beneficial effects as follows:
(1) preparation technology of the present invention is simple, and agarose had not only been made reducing agent but also used as stabilizers in preparation process, without introducing otherReducing agent or additive, safety non-toxic.
(2) Ago-Gel is better to the compatibility of nanogold particle, has solved in other preparation methods chemical reagent to nm of goldThe problem that Particle Phase capacitive is poor.
(3) internal cavities of Ago-Gel can be controlled the size of nanogold particle and prevent that nano Au particle from reuniting.
(4) in preparation process, adopt cryodesiccated method to remove gel, remove gel without heating or calcining. ColdIn the dry product obtaining of freeze-drying, impurity content is few, washs and can effectively remove impurity, without increasing complicated going with ultra-pure waterDeimpurity step.
(5) size uniform of nanogold particle in the nano-Au solution making, particle diameter is very little, reaches several nanometers, good stability,Difficult reunion.
(6) nano-Au solution making is taking water as solvent, and source is simple, cheap, nontoxic, and the nano-Au solution obtaining is usedSafety, convenient storage.
Brief description of the drawings
Below in conjunction with accompanying drawing, the invention will be further described, in accompanying drawing:
Fig. 1 is the uv-visible absorption spectra figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 3 is the particle size distribution figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 4 is the uv-visible absorption spectra figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Fig. 5 is the transmission electron microscope picture figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Fig. 6 is the particle size distribution figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Detailed description of the invention
For making object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, to the present inventionBe further elaborated. Should be appreciated that specific embodiment described herein is only in order to explain the present invention, and be not used in limitDetermine the present invention.
The material, the reagent etc. that in following embodiment, use if no special instructions, obtain in all can be from commercial channels.
In following embodiment, detect sample by ultraviolet-visible spectrophotometer (TU-1901 dual-beam ultraviolet-uisible spectrophotometer)Product characteristic absorption peak.
In following embodiment by transmission electricity electron microscope (JEM-2100) observing samples pattern.
In following embodiment, pass through particle size analyzer (dynamic light scattering/potentiometer PSSNicomp380) observing samples size distribution.
Embodiment 1:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, stir untilMixed liquor becomes clear, obtains uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirsMix 5min, the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process. Mixed solution is putIn 25 DEG C of placement 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water,Obtain described nano-Au solution.
Particle in the product that the present embodiment obtains is nanogold particle through ultraviolet-visible spectrophotometer Analysis deterrmination, its ultraviolet-visible absorption spectra figure is shown in Fig. 1. Transmission electron microscope results shows, the particle obtaining in product is spherical, and its SEM figure is shown in Fig. 2.Adopt particle size analyzer to analyze the size distribution state of particle in product, result shows, particle size is mainly distributed in 2～5nm,Average grain diameter is 3nm, and its particle size distribution figure is shown in Fig. 3.
Embodiment 2:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 5mL ultra-pure water, mixed liquor is placed in to water bath and heats, stir untilMixed liquor becomes clear, obtains uniform agarose solution;
(2) in the agarose solution of preparation, adding 5mL concentration is the chlorauric acid solution of 0.02mM, and at 90 DEG C, constant temperature stirsMix 4min, the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process. Mixed solution is putIn 20 DEG C of placement 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water,Obtain described nano-Au solution.
Particle in the product that the present embodiment obtains is nanogold particle by ultraviolet-visible spectrophotometer Analysis deterrmination, its purpleOutward-visible absorption spectra figure is shown in Fig. 4. Transmission electron microscope results shows, the particle obtaining in product is spherical, and its SEM figure is shown in Fig. 5.Adopt particle size analyzer to analyze the size distribution state of particle in product, result shows, particle size is mainly distributed in 2～5nm,Average grain diameter is 2.9nm, and its particle size distribution figure is shown in Fig. 6.
Embodiment 3:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 0.8g Ago-Gel and add in 8.5mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stirUntil mixed liquor becomes clear, obtain uniform agarose solution;
(2) in the agarose solution of preparation, adding 1.5mL concentration is the chlorauric acid solution of 2.5mM, and at 80 DEG C, constant temperature stirsMix 5min, the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process. Mixed solution is putIn 30 DEG C of placement 8d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water,Obtain described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 7～10nm, and average grain diameter is 8.3nm.
Embodiment 4
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.0g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stir straightTo mixed liquor change clear, obtain uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirsMix 3min, the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process. Mixed solution is putIn 25 DEG C of placement 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water,Obtain described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 2～7nm, and average grain diameter is 5.2nm.
Embodiment 5:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stir straightTo mixed liquor change clear, obtain uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirsMix 5min, the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process. Mixed solution is putIn 30 DEG C of placement 1d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step 2 being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water,Described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 0.2～1.4nm, and average grain diameter is 1nm.
Without prejudice to essence of the present invention and spirit in the situation that, those of ordinary skill in the art may make according to the present invention variousThe change of various kinds or distortion, but these corresponding changes or distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (6)
1. a preparation method for the nano-Au solution based on Ago-Gel, comprises the following steps:
(1) in water, add Ago-Gel, heat to obtain the uniform agarose solution of clarification;
(2) in agarose solution, add chlorauric acid solution, constant temperature stirs, and obtains reaction solution, and reaction solution normal temperature is putPut, obtain nm of gold gel; Described constant temperature whipping temp is 80～100 DEG C, and constant temperature mixing time is 3～5min, and normal temperature temperature is20～30 DEG C, normal temperature standing time is 1～15d;
(3) the nm of gold gel obtaining is carried out to freeze drying and remove gel, after washing, obtain described nano-Au solution; Nm of gold is moltenLiquid is dispersed in water and is formed by nanogold particle, and nanogold particle size uniform is controlled, and average grain diameter is 1～10nm.
2. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that,Described water is ultra-pure water.
3. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that,Described agarose solution and chlorauric acid solution volume ratio are (1～9): 1.
4. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that,The concentration of described chlorauric acid solution is 0.02～2.5mM.
5. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that,In described agarose solution, add after chlorauric acid solution, the concentration of agarose in gained mixed solution is 0.08～0.15g/mL.
6. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that,Described washing step is with ultra-pure water washing 3 times.
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| CN106180753B (en) * | 2016-08-05 | 2019-01-15 | 武汉工程大学 | A kind of preparation method of nano silver particles and thus obtained nano silver particles |
| CN106180752B (en) * | 2016-08-05 | 2018-05-08 | 武汉工程大学 | A kind of preparation method of dendroid silver |
| CN106346018B (en) * | 2016-09-21 | 2019-02-01 | 武汉工程大学 | A kind of preparation method and applications of agarose/nano silver plural gel |
| CN106645135B (en) * | 2017-02-27 | 2019-12-10 | 南京七彩生物科技有限公司 | preparation method of gold nanorod film and sensing application thereof |
| CN112059200B (en) * | 2020-08-21 | 2023-04-18 | 武汉纺织大学 | Silver nanoparticles and macro-controllable preparation method thereof |
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