CN102581299A - Photochemical preparation method of noble metal nanoparticles - Google Patents
Photochemical preparation method of noble metal nanoparticles Download PDFInfo
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- CN102581299A CN102581299A CN201210039470XA CN201210039470A CN102581299A CN 102581299 A CN102581299 A CN 102581299A CN 201210039470X A CN201210039470X A CN 201210039470XA CN 201210039470 A CN201210039470 A CN 201210039470A CN 102581299 A CN102581299 A CN 102581299A
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Abstract
The invention discloses a photochemical preparation method of noble metal nanoparticles. The photochemical preparation method comprises preparing a noble metal ion solution, preparing a light reductant, mixing the noble metal ion solution with the light reductant to form a mixed solution, providing a light source, and reducing noble metal clusters in the mixed solution by the light reductant throught illumination to obtain the noble metal nanoparticles. Compared with the conventional photochemical synthesis technology, the photochemical preparation method does not need to pre-synthesize seed crystals, so that a complicated seed crystal synthetic step in the photochemical synthesis technology can be saved. The noble metal nanoparticles prepared by the photochemical preparation method disclosed by the invention are good in size uniformity and stable in quality, and the instruments and the reagents are simple, the additional protectants and the reducers are not needed, so that the influence to environment is reduced, and the whole synthetic process is environmentally-friendly.
Description
[technical field]
The present invention relates to the preparation method of noble metal nano particles, relate in particular to a kind of photochemical method for preparation of noble metal nano particles.
[background technology]
Noble metal nano particles such as gold and silver is because have unique physicochemical properties, on sign, photoelectric subassembly, catalytic reaction and the SERS of antibiotic by being applied in widely, chemistry or biological sensing, cell or tissue image.
Have the method for noble metal nano particles such as synthetic gold of many kinds and silver to be developed, wherein, the wet chemistry method has the high gold of a large amount of preparation homogenieities and the characteristic of Nano silver grain.The wet chemistry method can be divided into electrochemical process, chemical reduction method, acoustic wave chemical method and photochemical method according to its composition principle.In these methods, photochemical method can be reached the purpose of reaction through irradiation daylight in theory, and is considered to have the friendly advantage of environment.Therefore, the Actinochemical synthesis of exploitation nano-noble metal can meet the continuous forever spirit of current Green Chemistry and environment in fact.
Utilize in the past in the technology of synthetic gold of photochemical method and Nano silver grain,, therefore need utilize chemical synthesis to produce suitably big or small metal nanoparticle earlier as crystal seed owing to need be sub with the surface plasma of light action.Traditional chemical method often need be used strong reductant; For example; Sodium borohydride (NaBH4); Reducing metal ion or metal misfit thing are obtaining crystal seed, but such crystal seed producing method can suffer from some problems: (1) strong reductant uses improperly, possibly cause to the operator or to the harm of ecology; (2) strong reductant need add the crystal seed that just can produce suitable size with suitable speed, and this operation technique needs patience and technology, and is prone to cause quality (kenel and the size distribution) instability of each batch nano particle; (3) produce the time-consuming program of taking a lot of work in this road of crystal seed owing to need to add reducing agent, the method suffers from the problem that can't produce in a large number.
[summary of the invention]
The technical problem that the present invention will solve provides a kind of synthetic crystal seed that do not need in advance, environmental protection, noble metal nano particles photochemical method for preparation simple to operate.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is that a kind of photochemical method for preparation of noble metal nano particles may further comprise the steps:
A) preparation one precious metal ion solution,
B) preparation one photo-reduction agent,
C) the mixed noble metal solion is mixed the formation mixed solution with the photo-reduction agent,
D) light source is provided, makes the noble metal group in the mixed solution bunch be reduced into noble metal nano particles by the photo-reduction agent through illumination.
The photochemical method for preparation of above-described noble metal nano particles, described precious metal ion solution is gold ion solution or silver ion solution.
The photochemical method for preparation of above-described noble metal nano particles, described gold ion solution is the tetra chlorauric acid aqueous solution, the molar concentration of the tetra chlorauric acid aqueous solution is 10
-2M-10
-3M; Described silver ion solution is a silver nitrate aqueous solution, and the molar concentration of silver nitrate aqueous solution is 5 * 10
-2M-5 * 10
-3M.
The photochemical method for preparation of above-described noble metal nano particles, described photo-reduction agent is a sodium citrate aqueous solution, the molar concentration of sodium citrate aqueous solution is 10
-2M-10
-3M.
The photochemical method for preparation of above-described noble metal nano particles, in step c), precious metal ion solution and sodium citrate aqueous solution mix with the magnetite agitator, and the molar concentration of precious metal ion is 10 in the mixed solution
-3-10
-5
The photochemical method for preparation of above-described noble metal nano particles, the molar concentration of precious metal ion is 5x10 in the mixed solution
-3M-10
-4M.
The photochemical method for preparation of above-described noble metal nano particles, described light source are LED, Halogen lamp LED, sodium vapor lamp or UV lamp, and the wavelength of light source is between 200 to 800nm, and in step d), the intensity of illumination on mixed solution surface is 1-60mW/cm
2
The photochemical method for preparation of above-described noble metal nano particles, the wavelength of light source are between 400 to 500nm, and in step d), the intensity of illumination on mixed solution surface is 20-60mW/cm
2
The inventive method is compared with traditional photochemistry synthetic technology, and following advantage is arranged:
(1) do not need synthetic in advance crystal seed; Make in the photochemistry synthetic technology that the crystal seed synthesis step of complicacy is able to omission; Utilize the prepared nano particle of the present invention to have good big or small homogeneity incessantly, and can synthesize gold, silver nano particle by the variation of optical source wavelength and the temperature of control reaction with difformity;
(2) instrument and the medicament of the synthesis step that uses of the inventive method and use are all comparatively simple, do not need extra interpolation protective agent and reducing agent, and alleviate the influence to environment, make more environmental protection of building-up process.
[description of drawings]
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is done further detailed explanation.
Fig. 1 is a cooking-pot type noble metal nano particles photochemistry synthetic method flow chart of the present invention.
Fig. 2 is the transmission electron microscope image of embodiment 1.
Fig. 3 is the uv-visible absorption spectroscopy figure of the sampling in time of embodiment 1.
Fig. 4 (A) and Fig. 4 (B) are the transmission electron microscope image of Nano silver grain after placement a period of time of embodiment 1.
Fig. 5 is the transmission electron microscope image of embodiment 2.
Fig. 6 is the transmission electron microscope image of embodiment 3.
Fig. 7 is the transmission electron microscope image of embodiment 4.
[specific embodiment]
Fig. 1 is one of the present invention cooking-pot type noble metal nano particles photochemistry synthetic method flow chart, mainly may further comprise the steps:
(a). prepare a precious metal ion solution,
(b). prepare a photo-reduction agent,
(c). mixed noble metal solion and photo-reduction agent form a mixed solution,
(d). mixed solution is controlled at specified temp,
(e). a light source is provided, makes the noble metal group in the mixed solution bunch be reduced into noble metal nano particles by the photo-reduction agent through illumination.
The precious metal ion solution of above-mentioned steps (a) comprises gold ion or silver ion, and ion source comprises tetra chlorauric acid (HAuCl4), silver nitrate (AgNO3) etc.Solvent can be ultra-pure water or deionized water.During preparation ion source is dissolved in the solvent and gets final product.
The photo-reduction agent of above-mentioned steps (b) is a natrium citricum, and in the present invention's the method, natrium citricum removes as the photo-reduction agent, also can be used as the required stabilizing agent of reaction and uses.
Aspect the photo-reduction agent; Under the situation that does not have citrate to exist; Irradiation can not make the reduction of silver ion or tetra chlorauric acid ion form nano particle, and under the situation of having only citrate and silver ion or tetra chlorauric acid ion to mix, a period of time still can not be observed the generation of metal nanoparticle at room temperature to keep solution; When light and citrate exist down simultaneously, its synergy just makes silver ion or tetra chlorauric acid ion be reduced into Yin Nami or gold nano crystal seed.But this synergy can be called " light is assisted the citrate reduction process " (photo-assisted citrate reduction process); In this process; Possibly be metal ion group bunch or citrate and the formed misfit thing of metal ion can with the visible light effect; Though the coefficient of its effect is very little, to such an extent as in the ultraviolet light visible light, can not present observable absorption value, however the energy of the group of only few part bunch or misfit photon that thing is caught; Just impel the reduction of citrate to produce, so citrate promptly is reduced into the nanometer crystal seed with metal ion down the auxiliary of light.The crystal seed that is produced with the general chemical reduction method of seed ratio that this method produced has more crystalline property, further again irradiation, and the preferable crystal seed of crystallinity promptly can see through the sub-media photochemical reaction of electricity slurry and grow up gradually.Because surface plasma and incident light effect produce the internal field of space anisotropic, impel the CONCENTRATION DISTRIBUTION of the ion in the surrounding liquid inhomogeneous, so this crystal can become to grow up to aspheric nanostructured.The kenel of these nanostructureds and size can see through modes such as control temperature and illumination wavelength and regulate and control.
On the other hand; The citrate ion that natrium citricum provides and other charged product can be adsorbed on surfaces of metal nanoparticles, make it electronegative; Thereby make nano particle identical and mutually exclusive because of electric charge, so can stable metal nano particle be suspended in the solution and avoid its gathering, deposition.
The temperature of above-mentioned steps (d) is controlled between 0 to 100 ℃, can adjust according to different embodiments.
The light source of above-mentioned steps (e) is by being provided by LED, Halogen lamp LED, sodium vapor lamp or UV lamp; The optical source wavelength that is used among the present invention is positioned between 200 to 800nm; Because of LED is the single wavelength light source supplier of the cheap and superior performance of a price; So the light source that is used by reaction with LDE lamp source for preferred embodiment enumerated because the electric field of the sub-formation of surface plasma has directionality, make the growth meeting presentation space of metal nanoparticle non-spare to growth; The optical source wavelength that provide this moment more can further be controlled the size and the shape of synthetic metal nanoparticle, therefore can give different wave length according to different embodiments and react.
The present invention's noble metal nano particles synthetic method can be enumerated 4 preferred embodiments explanation and fully understood by following, and makes and have common knowledge the knowledgeable in the art and can accomplish according to this.Right the present invention's enforcement kenel is not exceeded with the following example.
(a1) measure 17mg silver nitrate (AgNO3) powder with the electronics Libra, and be dissolved in evenly mixing in the 10ml deionized water (H2O), forming concentration is 10
-2The silver nitrate aqueous solution of M (mol/L).
(b1) measure the 1.32g natrium citricum with the electronics Libra, and be dissolved in evenly mixing in the 990ml deionized water (H2O), preparation 4.53x10
-3The M sodium citrate aqueous solution.
(c1) mix 10 of 1ml
-2The 4.53x10 of M silver nitrate aqueous solution and 99ml
-3The M sodium citrate aqueous solution also stirred 5 minutes with the magnetite agitator, and natrium citricum is fully mixed with silver nitrate, and concentration of silver ions is 10 in the solution at this moment
-4M.
(d1) mixed solution is positioned under the led light source that wavelength is 450nm, the intensity of illumination on mixed solution surface is about 20-60mW/cm
2, continuing irradiation, and reaction temperature is controlled at room temperature, solution becomes pink and promptly accomplishes reaction after about 1.5 hours.
The transmission electron microscope image of present embodiment gained is as shown in Figure 2; It is the Nano silver grain enlarged photograph for 12000 times of following findings of enlargement ratio; Can obviously find out by Fig. 2; The inventive method can obtain extremely how silver-colored decahedron nano particle on this embodiment, cording has the shape of particle selectivity and the size homogeneity of height.
Present embodiment solution colour change procedure sees also Fig. 3; It is the uv-visible absorption spectroscopy figure of sampling in time; Can be observed at 1.5 hours irradiation time solution and can have the highest 500nm absworption peak, this absworption peak is the major axis signal that silver-colored decahedron nano particle is provided.
Stable available Fig. 4 of the Nano silver grain that present embodiment is synthetic shows; Fig. 4 (A) is that the synthetic decahedron Nano silver grain of present embodiment is placed 2 months transmission electron microscope image; Fig. 4 (B) is that the synthetic decahedron Nano silver grain of present embodiment is placed the transmission electron microscope image in 1 year; Can see that it still has certain decahedron external form and size, show that the synthetic Nano silver grain of this method has good stable property.
Embodiment 2
(a2) measure 394mg tetra chlorauric acid (HAuCl4.3H2O) powder with the electronics Libra, and be dissolved in evenly mixing in the 100ml deionized water (H2O), forming concentration is 10
-2The tetra chlorauric acid aqueous solution of M.
(b2) measure the 1.32g natrium citricum with the electronics Libra, and be dissolved in evenly mixing in the 900ml deionized water (H2O), preparation 4.99x10
-3The M sodium citrate aqueous solution.
(c2) mix 10 of 10ml
-2The 4.99x10 of the M tetra chlorauric acid aqueous solution and 90ml
-3The M sodium citrate aqueous solution also stirred 5 minutes with the magnetite agitator, and tetra chlorauric acid is fully mixed with natrium citricum, and the GOLD FROM PLATING SOLUTION ion concentration is 10 at this moment
-3M.
(d2) mixed solution is positioned under the led light source that wavelength is 450nm, continues irradiation, the intensity of illumination on mixed solution surface is about 20-60mW/cm
2, and reaction temperature being controlled at room temperature, solution becomes redness and promptly accomplishes reaction after about 1.5 hours.
The transmission electron microscope image of present embodiment gained is as shown in Figure 5; It is the golden nanometer particle enlarged photograph for 20000 times of following findings of enlargement ratio; Can be found out obviously that by Fig. 5 the inventive method can obtain extremely many gold nano ball on this embodiment, its size is approximately on average about 10nm.
Embodiment 3
394mg tetra chlorauric acid (HAuCl4.3H2O) powder is measured with the electronics Libra in (a 3), and is dissolved in evenly mixing in the 100ml deionized water (H2O), and forming concentration is 10
-2The tetra chlorauric acid aqueous solution of M.
The 1.32g natrium citricum is measured with the electronics Libra in (b 3), and is dissolved in evenly mixing in the 900ml deionized water (H2O), preparation 4.99x10
-3The M sodium citrate aqueous solution.
(c3) mix 10 of 10ml
-2The 4.99x10 of the M tetra chlorauric acid aqueous solution and 90ml
-3The M sodium citrate aqueous solution also stirred 5 minutes with the magnetite agitator, and tetra chlorauric acid is fully mixed with natrium citricum, and the GOLD FROM PLATING SOLUTION ion concentration is 10 at this moment
-3M.
(d3) mixed solution is positioned under the led light source that wavelength is 638nm, the intensity of illumination on mixed solution surface is about 5-15mW/cm
2, continuing irradiation, and reaction temperature is controlled at room temperature, solution becomes redness and promptly accomplishes reaction after about 2.5 hours.
The transmission electron microscope image of present embodiment gained is as shown in Figure 6, can be learnt by Fig. 6, and the inventive method can obtain the average approximately golden nanometer particle about 20nm of size on this embodiment.
Embodiment 4
(a4) measure 39.4mg tetra chlorauric acid (HAuCl4.3H2O) powder with the electronics Libra, and be dissolved in evenly mixing in the 100ml deionized water (H2O), forming concentration is 10
-3The tetra chlorauric acid aqueous solution of M.
(b4) measure the 1.32g natrium citricum with the electronics Libra, and be dissolved in evenly mixing in the 900ml deionized water (H2O), preparation 4.99x10
-3The M sodium citrate aqueous solution.
(c4) mix 10 of 10ml
-3The 4.99x10 of the M tetra chlorauric acid aqueous solution and 90ml
-3The M sodium citrate aqueous solution also stirred 5 minutes with the magnetite agitator, and tetra chlorauric acid is fully mixed with natrium citricum, and the GOLD FROM PLATING SOLUTION ion concentration is 10 at this moment
-4M.
(d4) mixed solution is positioned under the led light source that wavelength is 356nm, the intensity of illumination on mixed solution surface is about 1-5mW/cm
2, continuing irradiation, and reaction temperature is controlled at room temperature, solution becomes redness and promptly accomplishes reaction after about 1.5 hours.
The transmission electron microscope image of present embodiment gained is as shown in Figure 7, and the inventive method can obtain the approximately on average golden nanometer particle about 25nm of size on this embodiment.
The above embodiment of the present invention is before photochemical reaction; The method does not need to make crystal seed with other chemical reduction method preparation, is the tetra chlorauric acid of light source irradiation silver nitrate and natrium citricum mixed solution or proper proportion and the mixed solution some time of natrium citricum can produce Nano Silver or nm of gold with sodium vapor lamp or LED lamp directly.The irradiation of starting stage can be induced citrate reduction silver ion and tetra chlorauric acid ion and formed silver or golden crystal seed respectively; Through the irradiation that continues, silver-colored or golden crystal seed can induce reduction process to become to grow up to good Nano Silver of crystallinity or nm of gold via electricity slurry.Utilize the prepared nano particle of the present invention to have good big or small homogeneity incessantly, and can synthesize gold, silver nano particle by the variation of optical source wavelength and the temperature of control reaction with difformity.
Comprehensive above-mentioned four preferred embodiments, the inventive method can provide the metal nanoparticle with height shape selectivity and size homogeneity, and has good stability, and the inventive method is compared with previous photochemistry synthetic technology, and following advantage is arranged:
(1) do not need synthetic in advance crystal seed; Make in the photochemistry synthetic technology that the crystal seed synthesis step of complicacy is able to omission; And the difference slightly that produces when removing because of the crystal seed building-up process, cause quality (kenel and the size distribution) instability of each batch metal nanoparticle;
(2) instrument and the medicament of the synthesis step that uses of the inventive method and use are all comparatively simple, do not need extra interpolation protective agent and reducing agent, and alleviate the influence to environment, make more environmental protection of building-up process.
Claims (8)
1. the photochemical method for preparation of a noble metal nano particles is characterized in that, may further comprise the steps:
A) preparation one precious metal ion solution,
B) preparation one photo-reduction agent,
C) the mixed noble metal solion is mixed the formation mixed solution with the photo-reduction agent,
D) light source is provided, makes the noble metal group in the mixed solution bunch be reduced into noble metal nano particles by the photo-reduction agent through illumination.
2. the photochemical method for preparation of noble metal nano particles according to claim 1 is characterized in that, described precious metal ion solution is gold ion solution or silver ion solution.
3. the photochemical method for preparation of noble metal nano particles according to claim 2 is characterized in that, described gold ion solution is the tetra chlorauric acid aqueous solution, and the molar concentration of the tetra chlorauric acid aqueous solution is 10
-2M-10
-3M; Described silver ion solution is a silver nitrate aqueous solution, and the molar concentration of silver nitrate aqueous solution is 5 * 10
-2M-5 * 10
-3M.
4. the photochemical method for preparation of noble metal nano particles according to claim 3 is characterized in that, described photo-reduction agent is a sodium citrate aqueous solution, and the molar concentration of sodium citrate aqueous solution is 10
-2M-10
-3M.
5. the photochemical method for preparation of noble metal nano particles according to claim 1 is characterized in that, in step c), precious metal ion solution and sodium citrate aqueous solution mix with the magnetite agitator, and the molar concentration of precious metal ion is 10 in the mixed solution
-3-10
-5
6. the photochemical method for preparation of noble metal nano particles according to claim 5 is characterized in that, the molar concentration of precious metal ion is 5x10 in the mixed solution
-3M-10
-4M.
7. the photochemical method for preparation of noble metal nano particles according to claim 1; It is characterized in that described light source is LED, Halogen lamp LED, sodium vapor lamp or UV lamp, the wavelength of light source is between 200 to 800nm; In step d), the intensity of illumination on mixed solution surface is 1-60mW/cm
2
8. the photochemical method for preparation of noble metal nano particles according to claim 1 is characterized in that, the wavelength of light source is between 400 to 500nm, and in step d), the intensity of illumination on mixed solution surface is 20-60mW/cm
2
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Cited By (12)
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|---|---|---|---|---|
| CN102921956A (en) * | 2012-11-01 | 2013-02-13 | 河南大学 | Method for preparing Au and Agx (Au) 1-x nano-crystals through organic phases |
| CN103480858A (en) * | 2013-09-10 | 2014-01-01 | 徐志兵 | Silver nano particle preparation method using visible light to reduce silver ions |
| CN105158229A (en) * | 2015-08-13 | 2015-12-16 | 南京理工大学 | Preparation method of high-sensitivity recyclable SERS (surface enhanced Raman spectroscopy) substrate |
| CN106964345A (en) * | 2016-12-31 | 2017-07-21 | 武汉理工大学 | A kind of noble metal porous nano film and preparation method thereof |
| CN107666975A (en) * | 2015-03-30 | 2018-02-06 | 印度科学工业研究所 | The method that the coated gold of biological organism and silver nano-grain are prepared with blue light |
| CN107837820A (en) * | 2017-11-21 | 2018-03-27 | 南京工业大学 | A kind of preparation method of two-dimentional MOFs material loads nano-particle |
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| CN113118432A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Noble metal nano particle and preparation method and application thereof |
| CN113118453A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Silver nano particle, preparation method thereof and photoinduction device |
| CN113118433A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Method for reconstructing morphology of noble metal nanoparticles |
| CN116440927A (en) * | 2023-04-25 | 2023-07-18 | 景德镇陶瓷大学 | Preparation method of silver-modified molybdenum sulfide nanoflower |
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| CN102921956A (en) * | 2012-11-01 | 2013-02-13 | 河南大学 | Method for preparing Au and Agx (Au) 1-x nano-crystals through organic phases |
| CN103480858A (en) * | 2013-09-10 | 2014-01-01 | 徐志兵 | Silver nano particle preparation method using visible light to reduce silver ions |
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| CN105158229A (en) * | 2015-08-13 | 2015-12-16 | 南京理工大学 | Preparation method of high-sensitivity recyclable SERS (surface enhanced Raman spectroscopy) substrate |
| CN106964345A (en) * | 2016-12-31 | 2017-07-21 | 武汉理工大学 | A kind of noble metal porous nano film and preparation method thereof |
| CN106964345B (en) * | 2016-12-31 | 2019-08-27 | 武汉理工大学 | A kind of noble metal porous nano film and preparation method thereof |
| CN107837820A (en) * | 2017-11-21 | 2018-03-27 | 南京工业大学 | A kind of preparation method of two-dimentional MOFs material loads nano-particle |
| CN113118453A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Silver nano particle, preparation method thereof and photoinduction device |
| CN113118432A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Noble metal nano particle and preparation method and application thereof |
| CN113118433A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Method for reconstructing morphology of noble metal nanoparticles |
| CN112191859A (en) * | 2020-09-29 | 2021-01-08 | 石河子大学 | Noble metal nano sol and preparation method and application thereof |
| CN112186199A (en) * | 2020-09-30 | 2021-01-05 | 中钢集团南京新材料研究院有限公司 | Catalyst for solid polymer fuel cell and preparation method thereof |
| CN112186199B (en) * | 2020-09-30 | 2022-02-08 | 中钢集团南京新材料研究院有限公司 | Catalyst for solid polymer fuel cell and preparation method thereof |
| CN116440927A (en) * | 2023-04-25 | 2023-07-18 | 景德镇陶瓷大学 | Preparation method of silver-modified molybdenum sulfide nanoflower |
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Application publication date: 20120718 |