CN101486101A - Method for preparing silver nano material with different appearance assisted with microwave - Google Patents
Method for preparing silver nano material with different appearance assisted with microwave Download PDFInfo
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Abstract
The invention discloses a method for synthesizing silver nanostructure materials with different shapes, and belongs to the technical field of preparation of nano materials. The invention provides a method and technology for synthesizing the silver nano materials with high efficiency, controllable shape and friendly environment. The method adds silver nitrate (or other salt containing silver such as silver acetate) into a reducing solution at room temperature and normal pressure, can grow and obtain the silver nanostructure materials with the different shapes through microwave treatment, and can achieve the aim of controlling the shape of products by controlling the mixture ratio and the reaction time of raw materials. The method can reduce the reaction cost and improve the production efficiency of the silver nano materials; and the prepared nano materials have the advantages of controllable shape, high purity, good structure and the like, and the method has good repeatability.
Description
Technical field
The present invention relates to field of nano material preparation, refer in particular to a kind of microwave auxiliary preparation of different-shape, the controlled silver nanostructured material method of shape.
Background technology
Current development of science and technology requires high integrated, the high density of ultramicronising, intellectuality, the element of material to store and characteristic such as ultrafast transmission provides wide space for the application of nanosecond science and technology and nano material.Nano science and nanometer technology are current one of the most great-hearted research fields, and two during the decade in the past, and the purpose of research will be used for nano material industrial production and daily life exactly veritably, really improves people's life.In nano material, because the physical features sizes such as coherence length of nano-grade size and optical wavelength, de Broglie wavelength and superconducting state quite or littler, make that the periodic boundary condition of crystal is destroyed; Near the superficial layer of nanoparticle atomic density reduces; The mean free path of electronics is very short, and locality and coherence strengthen.The atomicity that size decline also makes nanometer system comprise descends greatly, and fixing quasi-continuous can being with of macroscopic view be changed discrete energy level into.These cause the physical effect and the conventional material of sound, light, electricity, magnetic, heat, mechanics etc. of nano material macroscopic view different, are presented as quantum size effect, small-size effect, skin effect and macroscopical tunnel-effect etc.
Silver nano material is most important a kind of in the precious metal material, and it has extraordinary conduction and thermal conductivity, thereby becomes the emphasis of people's research.And, silver nanostructured because its special surface plasma effect is luminous in enhancing, medical science detects, there is very big application potential the bio-sensing aspect, and therefore, for preparing different-shape and different size silver nanostructuredly has very important theory and a practical value.The method for preparing at present nano material mainly contains template, hydro-thermal method, and the polyalcohol method, electrochemical methods etc. specifically can list of references: Chem.Commun., and 699 (1999), 700; Science, 294 (2001), 348; Chem.Material., 14 (2002), 4376; J.Phys.Chem.B, 108 (2004), 12877 etc.Above method all can prepare the ag material with nanostructured, but reaction condition is all very complicated, and the reaction time is very long, generally all needs 2～3 hours, and output is also relatively low; Maybe need to introduce other particle,, cause product impure as in course of reaction, adding nano platinum particle as catalyst.
Summary of the invention
The purpose of this invention is to provide a kind of microwave auxiliary preparation of different-shape, the controlled silver nanostructured material method of shape, with overcome the reaction condition complexity, the reaction time that exist among the existing preparation method long, yield poorly and defective such as product is impure.For this reason, the present invention by the following technical solutions, it may further comprise the steps:
(1), prepares argentiferous ion solution reaction system with silver nitrate or silver acetate powder and dispersant and join in the polyhydroxy liquid state organics;
(2) in this contains the solution reaction system of silver ion, add water soluble chloride, stir, obtain reacting precursor;
(3) adopt the method for microwave irradiation, this precursor irradiation under microwave that obtains is obtained the silver nano material of different-shape, the precursor of gained behind the microwave irradiation is obtained dark gray powder after washing, drying.
By above technical scheme, the beneficial effect that the present invention has is:
1) preparation method is simple, and cost is low, all can repeat to prepare high-quality nano silver wire in very wide Reaction conditions range;
2) this preparation method does not adopt metallic as catalyst, does not therefore introduce impurity.
Description of drawings
The stereoscan photograph of the silver nanostructured material of the different-shape of Fig. 1 embodiment 1 preparation;
The stereoscan photograph of the silver nanostructured material of the different-shape of Fig. 2 embodiment 2 preparations;
The stereoscan photograph of the silver nanostructured material of the different-shape of Fig. 3 embodiment 3 preparations;
The stereoscan photograph of the silver nanostructured material of the different-shape of Fig. 4 embodiment 11 preparations;
The XRD of the nano silver wire of Fig. 5 embodiment 2 preparations characterizes.
The specific embodiment
The present invention was divided into for two steps: at first being the precursor of preparation silver, is the ag material that obtains having nanostructured by microwave treatment then.Can reach the purpose of control product pattern by control reaction time and raw material proportioning.
One, the detailed process of the precursor of preparation silver is:
(1) with the silver nitrate of 100 weight portions or silver acetate with after the dispersant of 5～122 or 123～2000 weight portions evenly mixes, the mixed-powder that obtains is added in the polyhydroxy liquid state organics, and the ratio of the volume of this mixed-powder quality and polyhydroxy liquid state organics is 0.105:20 (g/ml)～0.3:20 (g/ml).When the even dispersing and dissolving of above-mentioned mixed-powder obtains the brown clear liquid behind the polyhydroxy liquid state organics, this clear liquid is argentiferous ion solution reaction system.
(2) in this contains the solution reaction system of silver ion, add water soluble chloride, add water soluble chloride quality be in the solution silver nitrate or silver acetate quality 0%～0.049% or 0.31%～13.2%; Obtain reacting precursor after stirring, this moment, solution changed the crineous suspension into.
In the said process, the silver nitrate and the silver acetate of the preferred purity of silver nitrate and acetic acid 〉=98%; Dispersant is polyvinylpyrrolidone (PVP), preferably polyethylene pyrrolidones (PVP, K 〉=30); The polyhydroxy liquid state organics is ethylene glycol or glycerine or both mixtures; Water soluble chloride is a sodium chloride, or magnesium chloride, or calcium chloride, or potassium chloride, wherein preferred sodium chloride.
Two, the detailed process that obtains having nanostructured silver by microwave treatment is:
Adopt the method for microwave irradiation, the precursor irradiation under microwave that obtains is obtained the yellowish-brown suspension, this suspension is obtained the silver-colored nanometer powder of grey black after washing, drying.
In the said process, microwave irradiation power is 240W～1200W, and microwave irradiation time is 1～10 minute; The suspension that obtains is through centrifugal or filter unnecessary organic matter is removed, and again with ethanol or aqueous dispersion and wash 1～2 time, promptly obtains silver-colored nanometer powder after the drying.
Set forth below by specific embodiment:
Embodiment 1:
Carry out according to preparation process.By mass ratio 1:0.05 the 0.2g silver nitrate is mixed adding with 0.01g PVP and fill in the beaker of 40ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.01g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 240W, 4.5min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, and is centrifugal once more, obtains the mixture of nano wire and nano particle behind the air drying.The sem test sample is that sample is sticked on the aluminium base sample platform, and Fig. 1 has provided the nano silver wire SEM photo that obtains according to embodiment 1.As can be seen from Figure 1, product is the mixture of nano wire and nano particle.
Embodiment 2:
Carry out according to preparation process.By mass ratio 1:1.22 the 0.18g silver nitrate is mixed adding with 0.22g PVP and fill in the beaker of 40ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.01g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 4.5min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 50ml aqueous dispersion and through supersound washing, and is centrifugal once more, the product air drying.The sem test sample is that sample is sticked on the aluminium base sample platform, and Fig. 2 has provided the nano silver wire SEM photo that obtains according to embodiment 2.As can be seen from Figure 2, the nano silver wire complete form for preparing, draw ratio is greater than 80; Fig. 5 is that the XRD of the nano silver wire of embodiment 2 preparation characterizes, nano silver wire perfect crystalline as can be seen from Figure 5, and do not contain impurity.
Embodiment 3:
Carry out according to preparation process.By mass ratio 1:2 the 0.2g silver nitrate is mixed adding with 0.4g PVP and fill in the beaker of 40ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.01g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 4.5min.Reaction back solution is removed redundant solution and is obtained solid through filtering.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, filters the product air drying once more.The sem test sample is that sample is sticked on the aluminium base sample platform, and Fig. 3 has provided the SEM photo of the silver-colored nanometer rods that obtains according to embodiment 3, and as can be seen from Figure 3, the length of silver-colored nanometer rods does not wait to 5 microns at 1 micron.
Embodiment 4
Carry out according to preparation process.By mass ratio 1:0.9 the 0.5g silver nitrate is mixed adding with 0.45g PVP and fill in the beaker of 65ml ethylene glycol, ultrasonic agitation 3～5 minutes obtains homogeneous transparent solution; Other adds 0.005g sodium chloride, continues ultrasonic agitation 2～3 minutes; The solution for preparing is put into micro-wave oven, and reaction condition is: 400W, 2min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 100ml aqueous dispersion and through supersound washing, and centrifugal once more, product air drying, product are nano silver wire.
Embodiment 5
Carry out according to preparation process.By mass ratio 1:0.9 the 0.5g silver nitrate is mixed adding with 0.45g PVP and fill in the beaker of 65ml ethylene glycol, ultrasonic agitation 3～5 minutes obtains homogeneous transparent solution; Other adds 0.002945g sodium chloride, continues ultrasonic agitation 2～3 minutes; The solution for preparing is put into micro-wave oven, and reaction condition is: 400W, 2min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 100ml aqueous dispersion and through supersound washing, and centrifugal once more, product air drying, product are Nano silver grain.
Embodiment 6
Carry out according to preparation process.By mass ratio 1:0.9 the 0.45g silver nitrate is mixed adding with 0.45g PVP and fill in the beaker of 60ml ethylene glycol, ultrasonic agitation 3～5 minutes obtains homogeneous transparent solution; The solution for preparing is put into micro-wave oven, and reaction condition is: 400W, 2min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 100ml aqueous dispersion and through supersound washing, and centrifugal once more, product air drying, product are Nano silver grain.
Embodiment 7
Carry out according to preparation process.By mass ratio 1:2 the 1g silver nitrate is mixed adding with 2g PVP and fill in the beaker of 200ml ethylene glycol, ultrasonic agitation 3～5 minutes obtains homogeneous transparent solution; Other adds 0.00147g sodium chloride, continues ultrasonic agitation 2～3 minutes; The solution for preparing is put into micro-wave oven, and reaction condition is: 400W, 2min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 100ml aqueous dispersion and through supersound washing, and centrifugal once more, product air drying, product are nano silver wire.
Embodiment 8
Carry out according to preparation process.By mass ratio 1:2 the 1g silver nitrate is mixed adding with 2g PVP and fill in the beaker of 200ml ethylene glycol, ultrasonic agitation 3～5 minutes obtains homogeneous transparent solution; Other adds 0.001g sodium chloride, continues ultrasonic agitation 2～3 minutes; The solution for preparing is put into micro-wave oven, and reaction condition is: 400W, 2min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is handled with the 100ml aqueous dispersion and through supersound washing, and centrifugal once more, product air drying, product are Nano silver grain.
Embodiment 9:
Carry out according to preparation process.By mass ratio 1:0.9 the 0.3g silver acetate is mixed adding with 0.27g PVP and fill in the beaker of 60ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains the homogeneous transparent precursor solution.To prepare solution and put into micro-wave oven, reaction condition is: 240W, 10min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, and is centrifugal once more, air drying.Product is the mixture of nano wire and nano particle.
Embodiment 10:
Carry out according to preparation process.By mass ratio 1:0.9 the 0.3g silver acetate is mixed adding with 0.27g PVP and fill in the beaker of 60ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains the homogeneous transparent precursor solution.To prepare solution and put into micro-wave oven, reaction condition is: 240W, 1min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, and is centrifugal once more, air drying.Product is a nano particle.
Embodiment 11:
Carry out according to preparation process.By mass ratio 1:1.22 the 0.18g silver nitrate is mixed adding with 0.22g PVP and fill in the beaker of 45ml glycerine, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds the 0.008g magnesium chloride, continues ultrasonic agitation 2～3 minutes; Be the yellow-white suspension this moment, is the precursor of preparation Nano silver grain.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 2.5min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is with 50ml ethanol or aqueous dispersion and process supersound washing processing, and is centrifugal once more, the product air drying.The sem test sample is that sample is sticked on the aluminium base sample platform, and Fig. 4 has provided the SEM photo of the Nano silver grain that obtains according to embodiment 11, and as can be seen from Figure 3, the form of Nano silver grain is mainly square, and particle diameter is evenly distributed.
Embodiment 12:
Carry out according to preparation process.By mass ratio 1:1.22 the 0.18g silver nitrate is mixed adding with 0.22g PVP and fill in the beaker of 45ml glycerine, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.009g calcium chloride, continues ultrasonic agitation 2～3 minutes; Be the yellow-white suspension this moment, is the precursor of preparation Nano silver grain.To prepare suspension and put into micro-wave oven, reaction condition is: 800W, 1min.Reaction back solution centrifugal 8min under the 4000r/min centrifugation rate.The solid that obtains is with 50ml ethanol or aqueous dispersion and process supersound washing processing, and is centrifugal once more, air drying.Product is the mixture of nano particle and nano wire.
Embodiment 13:
Carry out according to preparation process.By mass ratio 1:0.2 the 0.2g silver nitrate is mixed adding with 0.04g PVP and fill in the beaker of 45ml ethylene glycol and glycerine mixed liquor, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.0264g potassium chloride, continues ultrasonic agitation 2～3 minutes; Be the yellow-white suspension this moment, is the precursor of preparation Nano silver grain.To prepare suspension and put into micro-wave oven, reaction condition is: 400W, 3min.Reaction back solution is removed unnecessary liquid through filtering.The solid that obtains filters air drying once more with 50ml ethanol or aqueous dispersion and process supersound washing processing.Product is a nano wire.
Embodiment 14:
Carry out according to preparation process.By mass ratio 1:0.2 the 0.2g silver nitrate is mixed adding with 0.04g PVP and fill in the beaker of 45ml ethylene glycol and glycerine mixed liquor, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.0264g potassium chloride, continues ultrasonic agitation 2～3 minutes; Be the yellow-white suspension this moment, is the precursor of preparation Nano silver grain.To prepare suspension and put into micro-wave oven, reaction condition is: 1200W, 1min.Reaction back solution is removed unnecessary liquid through filtering.The solid that obtains filters air drying once more with 50ml ethanol or aqueous dispersion and process supersound washing processing.Product is a nano particle.
Embodiment 15:
Carry out according to preparation process.By mass ratio 1:1.23 the 0.2g silver nitrate is mixed adding with 0.246g PVP and fill in the beaker of 40ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.01g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 4.5min.Reaction back solution is removed redundant solution and is obtained solid through filtering.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, filters the product air drying once more.Product is a nano silver wire.
Embodiment 16:
Carry out according to preparation process.By mass ratio 1:10 the 0.1g silver nitrate is mixed adding with 1g PVP and fill in the beaker of 20ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.015g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 4.5min.Reaction back solution is removed redundant solution and is obtained solid through filtering.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, filters the product air drying once more.Product is the mixture of Nano silver grain and nano wire.
Embodiment 17:
Carry out according to preparation process.By mass ratio 1:20 the 0.3g silver nitrate is mixed adding with 6g PVP and fill in the beaker of 20ml ethylene glycol, ultrasonic agitation 5～10 minutes obtains homogeneous transparent solution; Other adds 0.012g sodium chloride, continues ultrasonic agitation 2～3 minutes; This moment, the suspension that is creamy white was the precursor of preparation nano silver wire.To prepare suspension and put into micro-wave oven, reaction condition is: 320W, 4.5min.Reaction back solution is removed redundant solution and is obtained solid through filtering.The solid that obtains disperses with 50ml water or ethanol and handles through supersound washing, filters the product air drying once more.Product is the mixture of Nano silver grain and nano wire.
Claims (7)
1, a kind of method of preparing silver nano material with different appearance assisted with microwave may further comprise the steps:
(1), prepares argentiferous ion solution reaction system with silver nitrate or silver acetate powder and dispersant and join in the polyhydroxy liquid state organics;
(2) in this contains the solution reaction system of silver ion, add water soluble chloride, stir, obtain reacting precursor;
(3) adopt the method for microwave irradiation, this precursor irradiation under microwave that obtains is obtained the silver nano material of different-shape, the precursor of gained behind the microwave irradiation is obtained dark gray powder after washing, drying.
2, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1, it is characterized in that the described dispersant of step (1) is polyvinylpyrrolidone (PVP), described polyhydroxy liquid state organics is the mixture of ethylene glycol or glycerine or ethylene glycol and glycerine.
3, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1, it is characterized in that the described water soluble chloride of step (2) is a sodium chloride, or magnesium chloride, or calcium chloride, or potassium chloride, and the addition of this water soluble chloride by: the quality of adding water soluble chloride be in the solution silver nitrate or silver acetate quality 0%～0.049% or 0.31%～13.2%.
4, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1, it is characterized in that step (1) and step (2) are: with the dispersant of the silver nitrate of 100 weight portions or silver acetate and 5～122 or 123～2000 weight portions evenly after, obtain mixed-powder and add in the polyhydroxy liquid state organics, the ratio of the volume of mixed-powder quality and polyhydroxy liquid state organics is 0.105:20 (g/ml)～6.3:20 (g/ml).
5, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1 is characterized in that used microwave irradiation power is 240W～1200W in the described step (3), and exposure time is 1～10 minute.
6, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1 is characterized in that the pattern of step (3) gained silver nano material has square shape Nano silver grain, near-spherical Nano silver grain, silver-colored nanometer rods and nano silver wire.
7, a kind of method of preparing silver nano material with different appearance assisted with microwave according to claim 1, it is characterized in that the described washing dry run of described step (3) for resulting silver nano material with different appearance through high speed centrifugation or filter, and then, obtain finished product after the drying with deionized water, absolute ethyl alcohol or acetone cleaning one to twice.
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