CN108161020A - A kind of octahedral preparation method of gold nano - Google Patents
A kind of octahedral preparation method of gold nano Download PDFInfo
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- CN108161020A CN108161020A CN201611144391.XA CN201611144391A CN108161020A CN 108161020 A CN108161020 A CN 108161020A CN 201611144391 A CN201611144391 A CN 201611144391A CN 108161020 A CN108161020 A CN 108161020A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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 present invention provides a kind of octahedral preparation methods of gold nano, belong to technical field of nano material.The present invention is in view of the shortcomings of the prior art; it is protective agent and pattern controlling agent to propose a kind of selection cationic surface active agent diallyl dimethyl ammoniumchloride (PDDA); in with pentanediol (PD) for the system of solvent and reducing agent, directly by gold chloride (HAuCl4) at high temperature a step reduction synthesis gold nano it is octahedra.The characteristic of the present invention is using cationic surface active agent, other any new chemical compositions and foreign ion are not introduced in system.This method is simple to operate, and repeatability and controllability are good, and the gold nano octahedron monodispersity for preparing synthesis is good, and particle size distribution is uniform, and the gold nano that can synthesize a variety of different size high-purities is octahedra.
Description
Technical field
The technical field prepared the present invention relates to gold nano-material more particularly to a kind of octahedral preparation side of gold nano
Method.
Background technology
The noble metal nanometer material of specific modality structure is since it is with small-size effect, skin effect, quantum size effect
Should wait makes its physical and chemical performance completely different from conventional blocks material.Currently, such material Industrial Catalysis, opto-electronic device,
Bio-sensing, imaging etc. have broad application prospects.The gold nano-material paid close attention in the present invention is noble metal nano material
Important one kind in material.Up to the present, the gold nano grain of different morphologies is successfully prepared synthesis, such as：Gold nanosphere, gold
Nanometer rods, nanowires of gold, gold nano bipyramid, gold-nano-piece, gold nano polyhedron etc..In contrast, stablize and prepare high yield
The gold nano octahedron particle of high-purity remains problem.Younan Xia research groups, Hyunjoon Song research groups,
Hicham Fenniri research groups etc., development improves the preparation synthesis octahedral method of gold nano, wherein mainly around more
First alcohol method and its modification method expansion.But these preparation methods, there are some shortcomings, the gold nano being prepared is octahedra
Dimensional homogeneity it is poor, yield is not high, impurity is more etc.；In preparation process, other metal impurities ions (Ag is often introduced+) or
Need gold kind so that the purity of product is affected to some extent, and preparation process complicates.
Even to this day, gold nano it is octahedral simple and it is controllable it is stable prepare synthesis remain one it is challenging
Work, strongly limits its application in each sciemtifec and technical sphere.Therefore, efficient stable synthesis size uniform, monodispersity be good, yield
The gold nano octahedron high with purity has very great significance to its practical application tool.
Invention content
In view of the deficienciess of the prior art, the present invention proposes a kind of selection cationic surface active agent polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is as protective agent and pattern controlling agent, in the system with pentanediol (PD) for solvent and reducing agent
In, directly by gold chloride (HAuCl under high temperature4) step reduction synthesis gold nano octahedron.The characteristic of the present invention is using sun
Ionic surfactant does not introduce other any new chemical compositions and foreign ion.This method is simple to operate, repeats
Property and controllability are good, and the gold nano octahedron monodispersity being prepared is good, particle size uniformity, and can synthesize a variety of differences
The high-purity gold nano of size is octahedra.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention provides a kind of octahedral preparation methods of gold nano, and described method includes following steps：
Step 1: at room temperature, by pentanediol (PD) precursor liquid, the cationic surface active agent polydiene of gold chloride
Diallyidimethylammonium chloride (PDDA) and a large amount of pentanediols (PD) are added separately in reaction vessel, are mixed evenly；
Step 2: then, specific steady temperature is maintained at by reaction process by heating equipment, when reacting specific
Between；
Step 3: last, the gold nano that high-purity is can obtain through centrifugation purification is octahedra.
Preferably, the molar concentration of pentanediol (PD) solution of the gold chloride is 20mM；The polydiene dimethylamine
The average molecular weight of ammonium chloride (PDDA) is 200000~300000；The pentanediol (PD) is 1,5-PD, and purity
>=97%.
Preferably, the amount of pentanediol (PD) solution of the gold chloride is 1mL；The diallyl dimethyl ammoniumchloride
(PDDA) amount is 0.08~3.2mL；The molar ratio of the gold chloride and diallyl dimethyl ammoniumchloride (PDDA) is 1：
(5~200)；The amount of a large amount of pentanediols (PD) is 10~50mL；It is highly preferred that the diallyl dimethyl ammoniumchloride
(PDDA) in 0.16~3.2mL, the molar ratio of gold chloride and diallyl dimethyl ammoniumchloride (PDDA) is 1 for amount control：
(10~200).If the amount of PDDA is very few, the control action of gold nano grain nucleating growth process is weakened, final product
There are the gold nano grain by-products of other patterns；If the amount of PDDA is excessive, to the pact of gold nano grain nucleating growth process
Shu Zuoyong is excessively strong, is unfavorable for forming gold nano octahedron.
Preferably, the reaction temperature is 200 DEG C~250 DEG C；The reaction time is 1min~5h.It is highly preferred that institute
The reaction time is stated as 5min~2h.If the reaction time is too short, the growth of gold nano octahedron particle is in nucleation stage, particle
Diameter is smaller and octahedral structure has not yet been formed.
Preferably, the reaction heating equipment selects accurate temperature controlling instruments, and the equipment carries the function of magnetic agitation,
Select thermostatical oil bath.
Preferably, the process of the centrifugation purification, using 10000~20000 revs/min of supercentrifuge of rotating speed, from
After the heart 30 minutes, centrifuge tube colourless solution at the middle and upper levels is removed, obtains precipitated product, ultrasonic disperse, repeated centrifugation purification is multiple, i.e.,
The gold nano that can obtain high-purity is octahedra.
Accurate control reaction condition of the invention, gives full play to diallyl dimethyl ammoniumchloride (PDDA) to particular crystal plane
Selective absorption acts on, and pentanediol (PD) is coordinated to have the collective effect of week reduction at high temperature, stablizes and prepares synthesis
The gold nano of high yield is octahedra.
Compared with prior art, the present invention has following advantageous effect：
1. simple to operate, repeatability and controllability are good, prepare the gold nano octahedron size uniform of synthesis, monodisperse
Property is good, by controlling reaction condition that can synthesize various sizes of gold nano octahedron material.Gold nano octahedron material is in water
With there is extraordinary dispersibility and stability in the solution such as ethyl alcohol, can for a long time preserve and not send out under the conditions of room temperature environment
It is raw to reunite.
2. present invention experiment prepares synthesis using one step of polyol process of improvement, conventional efficient is substantially increased, while
Reduce the error of pilot process.
3. gold nano octahedral precursor reactant growth phase does not introduce other any new chemical compositions and foreign ion, but
The preparation of various sizes of gold nano grain is realized only by regulation and control surfactant, reaction temperature and reaction time, and
The final octahedral purity of gold nano that synthesizes is up to more than 95%.
Description of the drawings
Fig. 1 (a) and Fig. 1 (b) is the scanning electron microscopy of gold nano octahedron particle prepared by the embodiment of the present invention 1 respectively
Mirror (SEM) figure and X-ray diffraction (XRD) figure；
Fig. 2 is scanning electron microscope (SEM) figure of gold nano octahedron particle prepared by the embodiment of the present invention 2；
Fig. 3 is scanning electron microscope (SEM) figure of gold nano octahedron particle prepared by the embodiment of the present invention 3；
Fig. 4 is scanning electron microscope (SEM) figure of gold nano octahedron particle prepared by the embodiment of the present invention 4；
Fig. 5 is scanning electron microscope (SEM) figure of gold nano octahedron particle prepared by the embodiment of the present invention 5；
Fig. 6 is scanning electron microscope (SEM) figure of gold nano octahedron particle prepared by the embodiment of the present invention 6.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, and following embodiment will be helpful to related neck
The technical staff in domain further understands the present invention, and the invention is not limited in following embodiments.
The present invention provides a kind of octahedral preparation method of gold nano, using cationic surface active agent polydiene third
Base alkyl dimethyl ammonium chloride (PDDA) is protective agent and pattern controlling agent, in the system with pentanediol (PD) for solvent and reducing agent
In, directly by gold chloride (HAuCl4) a step reduction synthesis at high temperature.
The diallyl dimethyl ammoniumchloride (PDDA, Mw=200000~300000,20wt%) that is used in the present invention,
Pentanediol (PD) and gold chloride (HAuCl4) directly bought from market, any purification process need not be done before.
According to the content of present invention, pentanediol (PD) solution for standby for the gold chloride that configuration molar concentration is 20mM.
Present disclosure is described in further detail with reference to specific embodiment, but the present invention is not limited to following acts
The specific examples of example.
Embodiment 1
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 0.8mL polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride (HAuCl4)
Molar ratio with diallyl dimethyl ammoniumchloride (PDDA) is 1：50；To be mixed to stir evenly, reaction solution is in micro- Huang at this time
Color, then by it, back flow reaction 30 minutes, cooled to room temperature obtain brown solution under the conditions of 220 DEG C of reaction temperatures；It will
Acquired solution supercentrifuge removes centrifuge tube colourless solution at the middle and upper levels after the centrifugation 30 minutes of 15000 revs/min of rotating speed,
The precipitated product for obtaining brown color is product gold nano octahedron granular materials.Gold nano manufactured in the present embodiment is octahedral
Shown in scanning electron microscope diagram such as Fig. 1 (a), the result shows that：Gold nano octahedron has good regular appearance degree and list
The characteristic of good dispersion, the average grain diameter of particle is 77.5nm, and particle diameter distribution accounts for about in 75~80nm, octahedra gold nano grain
More than 95% overall.The octahedral X-ray diffracting spectrum of gold nano (XRD) manufactured in the present embodiment such as Fig. 1 (b) is shown,
The result shows that：The nano particle prepared in experiment is face-centred cubic nanogold, it will be apparent that { 111 } diffraction peak illustrates Jenner
The octahedra oikocryst face presented of rice is { 111 } face.
Embodiment 2
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 0.8mL polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride (HAuCl4)
Molar ratio with diallyl dimethyl ammoniumchloride (PDDA) is 1：50；To be mixed to stir evenly, reaction solution is in micro- Huang at this time
Color, then by it, back flow reaction 30 minutes, cooled to room temperature obtain brown solution under the conditions of 200 DEG C of reaction temperatures；It will
Acquired solution supercentrifuge removes centrifuge tube colourless solution at the middle and upper levels after the centrifugation 30 minutes of 15000 revs/min of rotating speed,
The precipitated product for obtaining brown color is product gold nano octahedron granular materials.Gold nano manufactured in the present embodiment is octahedral
Scanning electron microscope diagram as shown in Fig. 2, itself the result shows that：Gold nano octahedron has good regular appearance degree and monodisperse
Property good characteristic, the average grain diameter of particle is 105nm, and particle diameter distribution accounts for totality in 100~110nm, octahedra gold nano grain
More than 90%.
Embodiment 3
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 0.16mL polydiene third
Base alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride
(HAuCl4) with the molar ratio of diallyl dimethyl ammoniumchloride (PDDA) it is 1：10；It is to be mixed to stir evenly, it reacts at this time
Liquid is in yellowish, and then by it, back flow reaction 30 minutes, cooled to room temperature obtain palm fibre under the conditions of 220 DEG C of reaction temperatures
Color solution；By acquired solution supercentrifuge after the centrifugation 30 minutes of 15000 revs/min of rotating speed, centrifuge tube is removed at the middle and upper levels
Colourless solution, the precipitated product for obtaining brown color are product gold nano octahedron granular materials.Jenner manufactured in the present embodiment
The octahedral scanning electron microscope diagram of rice as shown in figure 3, itself the result shows that：Gold nano octahedron has good regular appearance
Degree and the good characteristic of monodispersity, the average grain diameter of particle is 56nm, and particle diameter distribution is in 52~60nm, octahedra gold nano grain
Account for more than 95% overall.
Embodiment 4
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 1.6mL polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride (HAuCl4)
Molar ratio with diallyl dimethyl ammoniumchloride (PDDA) is 1：100；To be mixed to stir evenly, reaction solution is in micro- Huang at this time
Color, then by it, back flow reaction 30 minutes, cooled to room temperature obtain brown solution under the conditions of 220 DEG C of reaction temperatures；It will
Acquired solution supercentrifuge removes centrifuge tube colourless solution at the middle and upper levels after the centrifugation 30 minutes of 15000 revs/min of rotating speed,
The precipitated product for obtaining brown color is product gold nano octahedron granular materials.Gold nano manufactured in the present embodiment is octahedral
Scanning electron microscope diagram as shown in figure 4, itself the result shows that：Gold nano octahedron has good regular appearance degree and monodisperse
Property good characteristic, the average grain diameter of particle is 120nm, and particle diameter distribution accounts for totality in 115~125nm, octahedra gold nano grain
More than 95%.
Embodiment 5
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 0.8mL polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride (HAuCl4)
Molar ratio with diallyl dimethyl ammoniumchloride (PDDA) is 1：50；To be mixed to stir evenly, reaction solution is in micro- Huang at this time
Color, then by it, back flow reaction 5 minutes, cooled to room temperature obtain brown solution under the conditions of 220 DEG C of reaction temperatures；It will
Acquired solution supercentrifuge removes centrifuge tube colourless solution at the middle and upper levels after the centrifugation 30 minutes of 15000 revs/min of rotating speed,
The precipitated product for obtaining brown color is product gold nano octahedron granular materials.Gold nano manufactured in the present embodiment is octahedral
Scanning electron microscope diagram as shown in figure 5, itself the result shows that：Gold nano octahedron has good regular appearance degree and monodisperse
Property good characteristic, the average grain diameter of particle is 38nm, and particle diameter distribution accounts for overall in 35~41nm, octahedra gold nano grain
More than 95%.
Embodiment 6
Under agitation, by the gold chloride (HAuCl of 1mL4) pentanediol (PD) solution and 0.8mL polydiene propyl
Alkyl dimethyl ammonium chloride (PDDA) is respectively added in the round-bottomed flask for filling 30mL pentanediols (PD), wherein gold chloride (HAuCl4)
Molar ratio with diallyl dimethyl ammoniumchloride (PDDA) is 1：50；To be mixed to stir evenly, reaction solution is in micro- Huang at this time
Color, then by it, back flow reaction 2 hours, cooled to room temperature obtain brown solution under the conditions of 220 DEG C of reaction temperatures；It will
Acquired solution supercentrifuge removes centrifuge tube colourless solution at the middle and upper levels after the centrifugation 30 minutes of 15000 revs/min of rotating speed,
The precipitated product for obtaining brown color is product gold nano octahedron granular materials.Gold nano manufactured in the present embodiment is octahedral
Scanning electron microscope diagram as shown in fig. 6, itself the result shows that：Gold nano octahedron has good regular appearance degree and monodisperse
Property good characteristic, the average grain diameter of particle is 100nm, and particle diameter distribution accounts for overall in 95~105nm, octahedra gold nano grain
More than 95%.
Interpretation of result：
Above-described embodiment 1 and 2,3 and 4,5 and 6 result shows respectively：Quantity that reaction temperature, protective agent add in and anti-
The change of reaction conditions is waited between seasonable and causes the change of final size of nanometer gold grain.Therefore, item is reacted by accuracy controlling
Part, you can prepare the gold nano octahedron material of each size uniform in synthesis wider range.
Claims (7)
1. a kind of octahedral preparation method of gold nano, which is characterized in that described method includes following steps：
Step 1: at room temperature, by pentanediol (PD) precursor liquid, the cationic surface active agent polydiene propyl of gold chloride
Alkyl dimethyl ammonium chloride (PDDA) and a large amount of pentanediols (PD) reducing solution are added separately in reaction vessel, are mixed evenly；
Step 2: specific steady temperature, back flow reaction specific time are maintained at by heating equipment reaction process；
Step 3: last, the gold nano that high-purity is can obtain through centrifugation purification is octahedra.
2. the octahedral preparation method of gold nano according to claim 1, which is characterized in that the pentanediol (PD) is 1,
5- pentanediols, and purity is not less than 95%；The molar concentration of pentanediol (PD) solution of the gold chloride is 10~30mM；It is described
The average molecular weight of diallyl dimethyl ammoniumchloride (PDDA) is 200000~500000.
3. the octahedral preparation method of gold nano according to claim 1, which is characterized in that the pentanediol of the gold chloride
(PD) amount of solution is 1~5mL；The amount of the diallyl dimethyl ammoniumchloride (PDDA) is 0.08~3.2mL；Described penta
The amount of glycol (PD) is 10~50mL；Gold chloride and mole of diallyl dimethyl ammoniumchloride (PDDA) in the reaction solution
Than being 1：(1~200).
4. the octahedral preparation method of gold nano according to claim 1, which is characterized in that the pentanediol (PD) is anti-
Answer in system is both solvent and reducing agent；The diallyl dimethyl ammoniumchloride (PDDA) controls for protective agent and pattern
Agent.
5. the octahedral preparation method of gold nano according to claim 1, which is characterized in that the reaction temperature is 180
DEG C~300 DEG C；The reaction time is 1min~5h.
6. the octahedral preparation method of gold nano according to claim 1, which is characterized in that essence is selected in the reaction heating
True temperature controlling instruments, at the same time the equipment can be microwave heating equipment, thermostatical oil bath or electric heating with magnetic stirring function
Set.
7. the octahedral preparation method of gold nano according to claim 1, which is characterized in that the centrifugation purification process
In, the supercentrifuge that rotating speed is 5000~20000 revs/min, centrifugation time 10~30 minutes are selected, repeated centrifugation purifies more
After secondary, brown final product is obtained.
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| CN113109412A (en) * | 2021-03-12 | 2021-07-13 | 同济大学 | Portable field nicotine detection method based on gold nanoparticle modified screen-printed electrode |
| CN114433866A (en) * | 2022-01-29 | 2022-05-06 | 中国科学院长春应用化学研究所 | Method for synthesizing chiral gold nanoparticles |
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