CN103341635B - A kind of method preparing nanogold particle by laser generation aqueous electron - Google Patents
A kind of method preparing nanogold particle by laser generation aqueous electron Download PDFInfo
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- CN103341635B CN103341635B CN201310259797.2A CN201310259797A CN103341635B CN 103341635 B CN103341635 B CN 103341635B CN 201310259797 A CN201310259797 A CN 201310259797A CN 103341635 B CN103341635 B CN 103341635B
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Abstract
The invention discloses a kind of method preparing nanogold particle by laser generation aqueous electron, the method comprises the steps: that surfactant, organic molecule are put in water by step 1., after carrying out ultrasonic dissolution, it is configured to water-surfactant-organic molecule solution；Gold chloride dissolution of crystals is configured to chlorauric acid solution in water by step 2.；Water-surfactant-organic molecule solution and chlorauric acid solution are formed mixed solution by step 3. in proportion, add in flowing sample cell；Step 4. after pulse laser focusing, will irradiate mixed solution, and gold chloride is reduced by the aqueous electron of generation, and the recovery time is 5-10min, prepares nanogold particle。By changing laser energy size or changing the ratio of mixed solution, thus it is possible to vary the particle diameter of nanogold particle。The method is simple to operate, environmentally friendly, and obtained nanogold particle is in aqueous phase, it is easy to transfer。
Description
Technical field
The present invention relates to materials science field, especially a kind of method preparing nanogold particle by laser generation aqueous electron。
Background technology
Nanometer gold, namely the nano-particle of gold is referred to, its diameter is at 1-100nm, nanometer gold, with the bioaffinity of its good stability, small-size effect, skin effect, optical effect and uniqueness, has a wide range of applications in fields such as Industrial Catalysis, biological medicine, bioanalytical chemistry, food safety quickly detections。
The method preparing nanogold particle at present mainly has Physical and chemical method。In physical method, it is most commonly that vacuum vapour deposition, soft landing method, laser ablation etc.。Physical method principle is simple, and products obtained therefrom impurity is few, quality is high, its shortcoming be instrument and equipment requirement is higher, producing cost is expensive, the size and dimension of the nanogold particle prepared is wayward。Chemical method mainly has aqueous reaction reducing process, microemulsion method, phase transfer method etc., nanogold particle prepared by chemical method is minimum up to several nanometers, it is easily controlled, shortcoming is that the nanogold particle obtained not easily shifts and assembles, easily comprising impurity, easily assemble, and need to add more dispersant, stabilizer and reducing agent, environmental hazard is bigger。
Chinese invention patent application " a kind of method (application number: 201210499205.X utilizing laser preparation of nano metallic particles；Publication number: CN102962466A) "; the method, in noble gas cabin, irradiates deposition metallic film on the transparent substrate with laser, and metallic film is become gas-nano metallic particles by thermal evaporation; cools down by inert fluid, completes the preparation of nano-metal particle。The method can accurately control nanoparticle size, it is to avoid small nano-particle is reunited, but there is also certain defect, and as device is complicated, process is loaded down with trivial details, length consuming time。
Summary of the invention
In view of above-mentioned background, present invention aim at the preparation method providing a kind of new nanogold particle, the method is simple to operate, environmentally friendly, and obtained nanogold particle is in aqueous phase, it is easy to transfer。Obtained nanogold particle particle size range is relatively big, even particle size distribution。
In order to achieve the above object, the technical solution adopted in the present invention specifically includes following steps:
Surfactant, organic molecule are put in water by step 1., after carrying out ultrasonic dissolution, are configured to water-surfactant-organic molecule solution；
Gold chloride dissolution of crystals is configured to chlorauric acid solution in water by step 2.；
Water-surfactant-organic molecule solution and chlorauric acid solution are formed mixed solution by step 3. in proportion, add in flowing sample cell；
Step 4. after pulse laser focusing, will irradiate mixed solution, and gold chloride is reduced by the aqueous electron of generation, and the recovery time is 5-10min, prepares nanogold particle。
In above-mentioned preparation method, described surfactant concentration in water is higher than critical micelle concentration, it is possible to form micelle。Surfactant is anion surfactant, and its hydrophobic group is internally formed apolar regions at micelle, and hydrophilic group contacts formation hydrophilic region with water。
In above-mentioned preparation method, described organic molecule is dissolved in inside micelle。Water and organic molecule are excited by pulse laser, and moment ionizes out a large amount of free electron。From water produce free electron quickly with cation compound, just disappear。And the free electron in a short period of time (about 10 produced inside micelle-15S) in from micelle interior shifting to aqueous phase。This part electronics is under the obstruction of the micellar structure of surfactant, it is impossible to cation compound, aqueous phase can exist the long period (about 10-7-10-5S)。This part electronics is unnecessary in aqueous phase, quickly forms aqueous electron, it is possible to as the strong reductant in aqueous phase。
In above-mentioned preparation method, described gold chloride ionizes out hydrion (H in water+) and tetrachloro alloy ion (AuCl4 -), with aqueous electron as strong reductant reduce gold chloride equation be:
In above-mentioned preparation method, described pulse laser is femtosecond or nanosecoud pulse laser。By changing laser energy size or changing the ratio of mixed solution, thus it is possible to vary the productivity of aqueous electron, thus preparing various sizes of nanogold particle。
Advantages of the present invention and providing the benefit that:
1. the present invention utilizes pulse laser to excite water-surfactant-organic molecule solution to generate aqueous electron, aqueous electron productivity can reach 10%, the life-span of aqueous electron can reach for 200 nanoseconds to several milliseconds, high aqueous electron productivity and long electron lifetime make metallic compound be easy to be reduced, and the aqueous electron that is attached on nanogold particle is mutually exclusive, can effectively stop the agglomeration of nanometer gold, thus forming the nanogold particle of even particle size distribution。Obtained nanogold particle particle size range is relatively big, even particle size distribution。
2. the method that the aqueous electron reducing process that the present invention adopts produces nanogold particle, simple to operate, utilize pulse laser and common chemical reagent just can realize。
3. the method that the aqueous electron reducing process that the present invention adopts produces nanogold particle, the chemical reagent used includes surfactant and organic molecule, environmentally friendly, does not result in pollution。
4. the method that the aqueous electron reducing process that the present invention adopts produces nanogold particle, obtained nanogold particle is in aqueous phase, it is easy to transfer。
The present invention cannot be only used for the preparation of nanometer gold, it may also be used for the preparation of the material such as nanometer silver, Nanometer Copper, it is only necessary to gold chloride changes into corresponding silver or mantoquita or acid。
Accompanying drawing explanation
Fig. 1 is the schematic diagram of a kind of method being prepared nanogold particle by laser generation aqueous electron；
Fig. 2 is the uv-visible absorption spectra figure of the nanogold particle of embodiment 1 preparation；
Fig. 3 is the electron microscope picture of the nanogold particle of embodiment 1 preparation；
In accompanying drawing, 1. pulse laser, 2. surfactant, 3. organic molecule, 4. tetrachloro alloy ion, 5. water。
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail。
A kind of method preparing nanogold particle by laser generation aqueous electron as shown in Figure 1, it includes pulse laser 1, surfactant 2, organic molecule 3, tetrachloro alloy ion 4 and water 5。Described pulse laser 1 is femtosecond or nanosecoud pulse laser, and described surfactant 2 is anion surfactant, and concentration is higher than critical micelle concentration。Measure the absorption spectrum of obtained nanogold particle solution in following embodiment with ultraviolet/visible/near infrared spectrophotometer (Lambda1050), reference solution is the mixed solution of water-surfactant-organic molecule solution and chlorauric acid solution。
Embodiment 1:
By 66.14mg anion surfactant dodecyl sodium sulfate (molecular weight 272.38), 8.74mg organic molecule trans 1,2-stilbene (molecular weight 180.25) is put in 100mL water, carry out ultrasonic dissolution 5 minutes, be configured to water-surfactant-organic molecule solution。Chlorauric acid solution that 1mL mass fraction is 0.1% being mixed with 5mL water-surfactant-organic molecule solution and put in flowing sample cell, wherein the amount of substance ratio of surfactant, organic molecule and gold chloride is 5: 1: 1。Pulsewidth is 8ns, and repetition rate is 10Hz, and energy is that the ps pulsed laser and ns pulsed laser of 10mW is through lens focus, irradiation mixed solution 5-10min。Solution colour is shoaled red by light blue, eventually becomes redness, generates nanogold particle。
It is illustrated in figure 2 the uv-visible absorption spectra of the nanogold particle of embodiment 1, the absorption maximum of nanogold particle is at 516.5nm place, " resonance scattering spectroscopy of golden nanometer particle " paper reports a kind of luminosity scale measuring gold nano grain particle diameter, the maximum absorption wavelength of gold nano and the relation of particle diameter, have equation below d=(260 λmax-1.34×105)1/2。Its particle size range can be known by inference at 15-20nm according to formula。This is consistent with the electron microscope picture of nanogold particle prepared by the embodiment 1 shown in Fig. 3。
Embodiment 2:
By 33.07mg anion surfactant dodecyl sodium sulfate (molecular weight 272.38), 4.37mg organic molecule trans 1,2-stilbene (molecular weight 180.25) is put in 100mL distilled water, carry out ultrasonic dissolution 5 minutes, be configured to water-surfactant-organic molecule solution。Chlorauric acid solution that 1mL mass fraction is 0.1% being mixed with 5mL water-surfactant-organic molecule solution and put in flowing sample cell, wherein the amount of substance ratio of surfactant, organic molecule and gold chloride is 5: 1: 2。Pulsewidth is 8ns, and repetition rate is 10Hz, and energy is that the ps pulsed laser and ns pulsed laser of 10mW is through lens focus, irradiation mixed solution 5-10min。Solution colour is shoaled red by light blue, eventually becomes redness, generates nanogold particle。It is 40-50nm by the particle diameter of uv-visible absorption spectra and the nanogold particle of electron microscope picture confirmation generation。
Embodiment 3:
Compared with embodiment 1, except the energy of ps pulsed laser and ns pulsed laser is set to 20mW, other are identical with embodiment 1, are confirmed that by uv-visible absorption spectra and electron microscope picture the particle diameter of the nanogold particle produced is 10-16nm。
Embodiment 4:
Compared with embodiment 2, except the energy of ps pulsed laser and ns pulsed laser is set to 20mW, other are identical with embodiment 2, are confirmed that by uv-visible absorption spectra and electron microscope picture the particle diameter of the nanogold particle produced is 30-40nm。
Claims (3)
1. the method preparing nanogold particle by laser generation aqueous electron, it is characterized in that comprising the steps: that surfactant, organic molecule are put in water by step (1), after carrying out ultrasonic dissolution, it is configured to water-surfactant-organic molecule solution；Gold chloride dissolution of crystals is configured to chlorauric acid solution in water by step (2)；Water-surfactant-organic molecule solution and chlorauric acid solution are formed mixed solution by step (3) in proportion, add in flowing sample cell；Step (4) after pulse laser focusing, will irradiate mixed solution, and gold chloride is reduced by the aqueous electron of generation, and the recovery time is 5-10min, prepares nanogold particle；Described surfactant is dodecyl sodium sulfate, and described organic molecule is trans stilbene, and dodecyl sodium sulfate forms micelle in water, and trans stilbene is dissolved in inside micelle。
2. a kind of method preparing nanogold particle by laser generation aqueous electron according to claim 1, it is characterised in that: described pulse laser is femtosecond or ps pulsed laser and ns pulsed laser。
3. a kind of method preparing nanogold particle by laser generation aqueous electron according to claim 1, it is characterised in that: made nanogold particle particle diameter is within the scope of 5-50nm。
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| CN109868462A (en) * | 2019-03-28 | 2019-06-11 | 北京理工大学 | A method of realizing laser assisted gold ion electronation at the nanoscale |
| CN113649586A (en) * | 2021-07-12 | 2021-11-16 | 杭州苏铂科技有限公司 | Laser-assisted seedless gold nanostar synthesis method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1431039A (en) * | 2003-02-14 | 2003-07-23 | 中国科学院上海光学精密机械研究所 | Method for preparing metal sol under super-short pulse laser inducement |
| US20060057384A1 (en) * | 2004-04-01 | 2006-03-16 | Benoit Simard | Methods for the fabrication of gold-covered magnetic nanoparticles |
| CN101090785A (en) * | 2004-11-26 | 2007-12-19 | 首尔国立大学工业基金会 | Novel methods of large scale production monodisperse nano grain |
| CN102795596A (en) * | 2011-05-27 | 2012-11-28 | 中国科学院物理研究所 | Ultrafast laser pulse method for forming nanopores with diameters of 2 nanometers |
| CN102921961A (en) * | 2012-11-30 | 2013-02-13 | 南京大学 | Method for producing metallic nanomaterials through femtosecond lasers |
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| JP2008000654A (en) * | 2006-06-21 | 2008-01-10 | 3R Corp | Manufacturing method of nanoparticle with a particle size of 200 nm or less |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1431039A (en) * | 2003-02-14 | 2003-07-23 | 中国科学院上海光学精密机械研究所 | Method for preparing metal sol under super-short pulse laser inducement |
| US20060057384A1 (en) * | 2004-04-01 | 2006-03-16 | Benoit Simard | Methods for the fabrication of gold-covered magnetic nanoparticles |
| CN101090785A (en) * | 2004-11-26 | 2007-12-19 | 首尔国立大学工业基金会 | Novel methods of large scale production monodisperse nano grain |
| CN102795596A (en) * | 2011-05-27 | 2012-11-28 | 中国科学院物理研究所 | Ultrafast laser pulse method for forming nanopores with diameters of 2 nanometers |
| CN102921961A (en) * | 2012-11-30 | 2013-02-13 | 南京大学 | Method for producing metallic nanomaterials through femtosecond lasers |
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