CN104511597B - A kind of method for preparing gold nano grain - Google Patents
A kind of method for preparing gold nano grain Download PDFInfo
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- CN104511597B CN104511597B CN201510037346.3A CN201510037346A CN104511597B CN 104511597 B CN104511597 B CN 104511597B CN 201510037346 A CN201510037346 A CN 201510037346A CN 104511597 B CN104511597 B CN 104511597B
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- nano grain
- gold nano
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Abstract
The invention discloses a kind of method for preparing gold nano grain.The method is soaked in injector steel needles in chlorauric acid solution at room temperature using displacement reaction principle, can be prepared into gold nano grain after 1h.Different draw points is different from gold chloride reaction rate, and some draw points are contacted with gold chloride.The method is provided a kind of possible and there is preferable potential application ability for quickly preparing gold nano grain.The size of nanometer gold grain that the method is prepared in spherical and prism-shaped, has preferable potentiation between 20nm～50nm to Raman signal.The method has preferable application potential in surface enhanced raman spectroscopy application.
Description
Technical field
The present invention relates to a kind of convenient at room temperature method for preparing gold nano grain, belongs to nano material preparation technology neck
Domain.
Background technology
The precious metal material (such as gold, silver etc.) of nanoscale, catalytic property, electrical property, magnetic property and the light projected because of which
Property is learned, one of most dynamic study hotspot in nanosecond science and technology field is had become.Application with nano metal material
Further extensively, for the technology of preparing of nano metal material proposes requirements at the higher level.Nanometer wherein quickly can be prepared at normal temperatures
The method of granule is also one of research direction.In terms of biological applications, gold nano grain is with its preferable bio-compatibility
Receive much concern.For the synthesis of gold nano grain, there is all multi-methods.
It is to utilize principle of oxidation and reduction to prepare the conventional method of gold nano grain, by gold chloride (HAuCl4) in
AuCl4 -It is reduced into Au.The reducing agent being typically used for includes sodium citrate, shitosan etc..Using reduction of sodium citrate gold chloride, need
To realize under conditions of seething with excitement and being stirred vigorously.The reproducibility of shitosan is weaker, needs to realize at relatively high temperatures reducing.?
In micro-fluidic chip application, there is researcher to propose to use the firming agent of residual in silicone rubber (PDMS) as reducing agent, by chlorine gold
Acid and PDMS co-cultivation 24 hours or 48 hours, gold nano grain will be grown in being formed in PDMS surfaces or embedded PDMS multiple
Close structure.
Above method has some limitations, and preparation process is relatively complicated.Except utilizing principle of oxidation and reduction
Prepare outside gold nano grain, it is also possible to prepare gold nano grain using displacement reaction.Displacement reaction is using living between metallic element
The difference of dynamic property order, can prepare more inactive metal simple-substance with fast reaction.It is suitable that gold element comes movable metallic
The end of sequence, it is meant which is least active.Therefore gold nano grain can be prepared into by replacing reaction.Existing utilization is put
Changing reaction and preparing metallic particles, its main direction of studying is hollow metal nanoparticle knot to be prepared using displacement reaction
Structure, or form nanometer basket structure.Also document report prepares the Argent grain of tufted using aluminium foil and Argentous fluoride reaction.
Content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention provides a kind of gold nano grain for preparing
Method, the gold nano grain that the method is prepared are in spherical and prism-shaped, and its Raman scattering effect is strong, manufacture method simple,
Overcome the relatively complicated problem of current gold nano grain preparation process.
For achieving the above object, the technical solution used in the present invention is：A kind of method for preparing gold nano grain, using putting
Reaction principle is changed, draw point is contacted with chlorauric acid solution, you can reaction obtains gold nano grain.
Comprise the following steps：
Step one, draw point is immersed in chlorauric acid solution；
Step 2, reaction certain time after take out draw point, reacted solution is centrifuged, the precipitation obtained after centrifugation
Thing is gold nano grain.
Preferably：The time that the reaction temperature is reacted in -10-40 degree, the step 2 is 1 hour.
Specifically include following steps：
Step 1), at room temperature, the Deca chlorauric acid solution toward centrifuge tube；
Step 2), injector steel needles are soaked in ethanol and are cleaned with ultrasound wave, cleaning finish after, draw point is dried, so
Afterwards by drying after injector steel needles immersion centrifuge tube in chlorauric acid solution in；
Step 3), reaction take out draw point after a period of time, and reacted solution is centrifuged；
Step 4), the precipitate that obtains is gold nano grain after centrifugation；Which is scattered in deionized water again.
Preferably：The step 1) in Deca chlorauric acid solution concentration be 0.4%-0.6%, volume be 250-350 μ
L.
Preferably：The step 2) in injector steel needles be soaked in ethanol and clean 15-25min with ultrasound wave, after in 50-
Dry in 70 DEG C of baking ovens.
Preferably：The step 3) in reacted solution is centrifuged with the speed of 8000r/min-10000r/min
5-15min.
Preferably：The step 4) in deionized water volume be 250-350 μ L.
Preferably：Response time in the step 3 is 1 hour.
A kind of method for preparing gold nano grain that the present invention is provided, compared to existing technology, has the advantages that：
1st, there is displacement reaction using draw point and gold chloride in the present invention, can quickly prepare gold nano at normal temperatures
Grain.Compared with traditional method, maximum advantage is simple and quick.Distinct temperature is not needed to require, it is not required that specific examination
Agent, only need to be immersed in draw point in chlorauric acid solution, and the response time is shorter.
2nd, the gold nano grain that the present invention is prepared has preferably to strengthen to Raman scattering and makees in spherical and prism-shaped
With.
Description of the drawings
Fig. 1 is that draw point is soaked in chlorauric acid solution response situation schematic diagram after 1h；
Fig. 2 is that centrifugation is precipitated thing and is scattered in again 300 μ L deionized water schematic diagrams；
Fig. 3 is gold nano grain solution Spectral Extinction；
Fig. 4 is gold nano grain transmission electron microscope (TEM) phenogram；
Fig. 5 is Raman signal enhancing figure of the gold nano grain to Raman molecular R6G；
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further described.
Embodiment 1
A kind of method for preparing gold nano grain：Using displacement reaction principle, draw point is contacted with chlorauric acid solution, you can
Reaction obtains gold nano grain.
Comprise the following steps：
Step one, draw point is immersed in chlorauric acid solution；
Step 2, reaction certain time after take out draw point, reacted solution is centrifuged, the precipitation obtained after centrifugation
Thing is gold nano grain.
The time that the reaction temperature is reacted in -10-40 degree, the step 2 is 1 hour.
Specifically include following steps：
Step 1), at room temperature, toward centrifuge tube 250 μ L concentration of Deca be 0.6% chlorauric acid solution；
Step 2), injector steel needles are soaked in ethanol cleaned with ultrasound wave 15min, after cleaning is finished, draw point is put
In 50 DEG C of baking ovens dry, then by drying after injector steel needles immersion centrifuge tube in chlorauric acid solution in；
Step 3), reaction take out draw point after 45 minutes, and reacted solution is centrifuged with the speed of 8000r/min
15min；
Step 4), the precipitate that obtains is gold nano grain after centrifugation；Which is scattered in 250 μ L deionized waters again
In.
Embodiment 2
Specifically include following steps：
Step 1), at room temperature, toward centrifuge tube 300 μ L concentration of Deca be 0.4% chlorauric acid solution；
Step 2), injector steel needles are soaked in ethanol cleaned with ultrasound wave 25min, after cleaning is finished, draw point is put
In 70 DEG C of baking ovens dry, then by drying after injector steel needles immersion centrifuge tube in chlorauric acid solution in；
Step 3), reaction take out draw point after 1 hour, and reacted solution is centrifuged with the speed of 10000r/min
5min；
Step 4), the precipitate that obtains is gold nano grain after centrifugation；Which is scattered in 300 μ L deionized waters again
In.
In order to the present invention is more preferably described, an example of the present invention is now enumerated.
The draw point head of syringe is chosen, is dipped in the middle of 300 μ L, 0.5% chlorauric acid solutions.Draw point is taken out after 1h, will
Solution is centrifuged, exhaust supernatant.Take bottom sediment to be scattered in 300 μ L deionized waters again.Finally to obtaining
Gold nano grain carry out various ways sign, including Spectral Extinction, transmission electron microscope (TEM) and Raman spectrum etc..
A kind of method for preparing gold nano grain：Draw point is immersed in chlorauric acid solution, reaction is obtained Jenner in 1 hour
Rice grain.The gold nano grain of the present invention has prismatic structures, differs in size, and major part is between 20nm～50nm.
Concrete preparation method is comprised the following steps：
Step 1). 300 μ L of Deca, 0.5% chlorauric acid solutions in 1.5mL centrifuge tubes；
Step 2). the injector steel needles immersion chlorauric acid solution after ethanol ultrasound wave is cleaned 20 minutes；
Step 3) draw point is taken out after .1 hours, and reacted solution is centrifuged.Rotating speed is 9000r/min, centrifugation
10 minutes；
Step 4). discarded yellow supernatant (unreacted chlorauric acid solution), precipitate is gold nano grain.Which is heavy
Newly it is scattered in 300 μ L deionized waters, subsequently to characterize (characterization method such as Spectral Extinction, TEM, SERS reinforced effects) to which.
The experiment parameter that is taken in above example is adjustable, it is not limited to this.
Concrete process is as follows：
1) draw point is cleaned.Draw point is soaked in ethanol ultrasound wave cleaning 20min, after dry in 60 DEG C of baking ovens.
2) draw point is soaked.As shown in figure 1, cleaned draw point is immersed in 300 μ L, 0.5% chlorauric acid solutions, in room temperature
Lower reaction 1h.
3) nano-particle is centrifuged to obtain.Draw point is taken out, centrifugation 10min is carried out with the speed of 9000r/min to solution, abandoned yellow
Color supernatant, precipitation is redissolved in 300 μ L deionized waters.As shown in Fig. 2 solution is in aubergine.
4) nano-particle is characterized.The nanoparticles solution for preparing is characterized with ultraviolet-visible absorption spectroscopy instrument.
From Fig. 3 Spectral Extinctions, which has obvious gold nano grain characteristic peak at 553nm.
5) gold nano grain morphology characterization.Table is carried out to the gold nano grain pattern for preparing with transmission electron microscope
Levy, as shown in figure 4, the nanoparticle size for preparing is in 20nm～50nm or so, and have spherical and polygon prism pattern special
Levy.
6) nano-particle application.Take 5 μ L gold nano grains solution to mix with 5 μ L R6G solution, test under water phase state
Raman signal.5 points are surveyed, its meansigma methods is taken.
7) as shown in figure 5, potentiation of the nanoparticle for preparing in the embodiment to R6G Raman signals.Can see
Go out in the presence of having gold nano grain, R6G Raman signals are significantly increased.The nano-particle has in terms of surface enhanced raman spectroscopy
Larger application potential.
From the foregoing, there is displacement reaction using the relatively active element in draw point and gold chloride in the present invention, can be normal
Gold nano grain is prepared quickly under temperature, the gold nano grain is in spherical and prism-shaped, there is preferably increasing to Raman scattering
Pretend use.The gold nano grain that the present invention is prepared is in spherical and prism-shaped, with existing document report difference, equally may be used
Surface enhanced raman spectroscopy is applied to, and effect is preferable.Compared with traditional method, maximum advantage is simple and quick.It is not required to
Want distinct temperature to require, it is not required that specific reagent, only draw point need to be immersed in chlorauric acid solution, and the response time compared with
Short.
The above is only the preferred embodiment of the present invention, it should be pointed out that：Ordinary skill people for the art
For member, 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
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of method for preparing gold nano grain, it is characterised in that：Using displacement reaction principle, by injector steel needles and chlorine gold
Acid solution is contacted, you can reaction obtains gold nano grain, and the gold nano grain is in spherical and prism-shaped.
2. the method for preparing gold nano grain according to claim 1, it is characterised in that comprise the following steps：
Step one, injector steel needles are immersed in chlorauric acid solution；
Step 2, reaction certain time after take out draw point, reacted solution is centrifuged, the precipitate obtained after centrifugation
As gold nano grain.
3. the method for preparing gold nano grain according to claim 2, it is characterised in that：The temperature of the reaction is in -10-
40 degree, the time that reacts in the step 2 is 1 hour.
4. the method for preparing gold nano grain according to claim 3, it is characterised in that：
Step 1）, at room temperature, the Deca chlorauric acid solution toward centrifuge tube；
Step 2）, injector steel needles are soaked in ethanol and are cleaned with ultrasound wave, cleaning finish after, draw point is dried, then will
In the chlorauric acid solution in injector steel needles immersion centrifuge tube after drying；
Step 3）, reaction take out draw point after a period of time, and reacted solution is centrifuged；
Step 4）, the precipitate that obtains after centrifugation be gold nano grain；Which is scattered in deionized water again.
5. the method for preparing gold nano grain according to claim 4, it is characterised in that：The step 1）The chlorine of middle Deca
The concentration of auric acid solution is 0.4%-0.6%, and volume is 250-350 μ L.
6. the method for preparing gold nano grain according to claim 5, it is characterised in that：The step 2）Middle syringe steel
Pin is soaked in ethanol and cleans 15-25min with ultrasound wave, after in 50-70 DEG C of baking oven dry.
7. the method for preparing gold nano grain according to claim 6, it is characterised in that：The step 3）In to reaction after
Solution centrifugation 5-15min is carried out with the speed of 8000r/min-10000r/min.
8. the method for preparing gold nano grain according to claim 7, it is characterised in that：The step 4）Middle deionized water
Volume be 250-350 μ L.
9. the method for preparing gold nano grain according to claim 8, it is characterised in that：The step 3）In reaction when
Between be 1 hour.
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| CN109128216A (en) * | 2018-10-26 | 2019-01-04 | 启东科赛尔纳米科技有限公司 | The synthetic method of gold nanoparticle under room temperature |
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| CN1159125C (en) * | 2002-05-27 | 2004-07-28 | 中国科学院长春应用化学研究所 | Process for preparing metallic nanoparticles with redox activity |
| CN1483539A (en) * | 2003-07-29 | 2004-03-24 | 中国科学院上海光学精密机械研究所 | Method for preparing metal nano material by means of metal displacement reaction |
| US8361188B2 (en) * | 2009-04-03 | 2013-01-29 | Indian Institute Of Science | Methods for preparing metal and metal oxide nanoparticles |
| CN203565874U (en) * | 2013-10-10 | 2014-04-30 | 金川集团股份有限公司 | Device for displacing and extracting copper powder from copper-bearing solution |
| CN104259451A (en) * | 2014-09-16 | 2015-01-07 | 南京航空航天大学 | Tubular structure gold nanometer materials and production method thereof |
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