CN102211205A - Method for preparing series of high-purity silver nanometer materials - Google Patents
Method for preparing series of high-purity silver nanometer materials Download PDFInfo
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Abstract
The invention relates to a method for preparing series of high-purity silver nanometer materials. The method comprises the following steps: using a halogen-containing metal salt adjuvant to treat polyalcohol, a macromolecule surface active agent, the halogen-containing metal salt adjuvant and salts of silver ions in three steps, and then preparing the nanometer materials by performing a hybrid reaction at a high temperature. The nanometer materials prepared by the using the method have the advantages of uniform appearance, high purity, excellent monodispersity, lower cost, and simple reaction device. By using the method, the appearance is controllable, the size controlling scope is wide, and the large-scale synthesis of silver nanometer materials can be realized. The method has an industrialization prospect.
Description
Technical field
The present invention relates to a kind of preparation method of silver nano material, specially refer to the preparation method of the serial silver nano material of a kind of pattern that can be used for chemistry and electrochemical catalysis, chemical sensor, biomolecule sensor, optical information storage, solar cell etc., controllable size.
Background technology
Along with the transformation of using energy source pattern, the development and use of solar cell especially of new generation are had higher requirement to the use with high conductivity, high successional metal nano material, as copper nano material, silver nano material.There has been several different methods to prepare the synthetic of copper nano material, particularly copper nano-wire at present, such as chemical vapour deposition (CVD) (Kim, C.; Gu, W.; Briceno, M.; Robertson, I.M.; Choi, H.; Kim, K.Adv.Mater.2008,20,1859-1863), in the aqueous systems be that the solution of reducing agent is combined to (Chang, Y. with the hydrazine hydrate; Lye, M.L.; Zeng, H. C.Langmuir 2005,21,3746-3748).Yet some character of copper itself have limited the application of its nanoscale material, because the copper nano material is active high, make to be difficult to the very easily oxidation of copper nano material store, and are not easy to use of large-scale production.In metal material, silver has thermal conductivity and the electric conductivity higher than copper, and has overcome the easy oxidation of copper nano material, the difficult shortcoming that stores.Because silver nano material has unique optics, electromagnetism, mechanics, catalytic performance, make its aspect such as electric slurry, electrically-conducting paint, electrically conductive ink, conductive rubber, conductive plastics and electromagnetic screen coating in various fields such as chemical-biological sensing, dimension nano circuit, molecular device, opto-electronic device, flexible electronic device, solar cell and electronics industry that important role be arranged.
At present, the method for synthetic silver nano material mainly contains template and wet chemistry synthetic method.Template mainly is divided into hard template and two kinds of approach of soft template.Hard template is a template with Woelm Alumina, CNT, aeroge etc. usually, prepares silver nano material by modes such as electro-deposition, chemical depositions; The soft template rule is to be template with the high molecular surfactant, prepare all kinds of silver nano materials with chemical reduction method again, the advantage that adopts template be can strict control silver nano material size, pattern, be controlled by pattern, size that template itself is had again, this has just proposed higher requirement to synthetic template, and these class methods exist the problem that template is removed toward contact simultaneously.The wet chemistry synthetic method is the main method that is used to prepare silver nano material at present.The Catherine Murphy of U.S. South Carolina university has reported (Caswell, K.K. under alkali condition; Bender, C.M.; Murphy, C.J.Nano Lett.2003,3,667-669.), and the nano silver wire of synthetic about 50 nanometers of diameter when not having other organic reagents, this method is simple, environmental protection, but the synthetic product dispersiveness is relatively poor, purity is relatively low.In addition, Chinese patent ZL200810019828.6 is then with the solution phase synthesi, synthesized nano silver wire under microwave condition in a large number, apace, the outstanding advantage of this method is exactly easy to be quick, but the synthetic nanowire diameter of this method changes greatly, purity is not high, pattern is even inadequately.200710046510.2 of Chinese patent application are with pyroreaction reflux mass-synthesis of silver nano material under inert gas shielding; the advantage of this method is can the mass-synthesis of silver nano material; yet the problem that this method exists is a back flow reaction device complexity; reaction needs inert gas shielding simultaneously, and this just makes the cost of this method increase greatly.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of method for preparing serial high-purity silver nano material, the silver nano material purity height of this method preparation, pattern is even, monodispersity good, and method is easy, cost is low.
The technical scheme that the present invention takes is:
A kind of method for preparing serial high-purity silver nano material comprises that step is as follows:
(1) polyalcohol, high molecular surfactant, halogen-containing slaine assistant are stirred or ultrasonic dissolution, get mixed solution A;
(2) salt with polyalcohol and silver ion dissolves through stirring or shaking, and gets mixed solution B;
(3) add an amount of polyalcohol in reactor, adopt ultrasonic mode of heating heating 5～60 minutes, add certain water gaging again, the continuation sonic oscillation also heated 1～30 minute;
(4) mixed solution A and B are added drop-wise in the aforesaid reaction vessel, with the reactor sealing, are positioned over high temperature furnace then and descend and kept 10～1000 minutes for interior 100～600 ℃ after being added dropwise to complete.
Above-mentioned halogen-containing slaine assistant is the mixture (arbitrary proportion) of one or more and mantoquita in KBr, zinc chloride, sodium chloride, potassium chloride, iron chloride, sodium bromide, KI, the sodium iodide.
Described mantoquita is one or more in copper bromide, copper chloride, copper nitrate, copper sulphate, the copper acetate.
The preferred KBr of described halogen-containing slaine assistant mixes with mol ratio with copper chloride at 1: 1.
Above-mentioned steps (1), (2), preferred 1: 1: 1 of the usage ratio of polyalcohol in (3) three steps.
The usage ratio of polyalcohol, high molecular surfactant is 5～1000: 0.01～50 (ml: g), promptly per 5～1000ml polyalcohol is with high molecular surfactant 0.01～50g in the step (1); Preferred 10～500: 0.1～25 (ml: g); High molecular surfactant and halogen-containing slaine assistant mass ratio are that 0.01～50: 0.05～100 (g: mg), promptly mass ratio 10～50000: 0.05～100.
The usage ratio of the salt of polyalcohol and silver ion pass is 5～1000 in the step (2): 0.01～50 (ml: g), preferred 10～500: 0.1～25 (ml: g).The volume ratio of polyalcohol and water is 5～1000: 10～500 in the step (3); Preferred 10～500: 0.1～20.
The preferred syringe pump propulsion mode of the described dropping of step (4) drips, and syringe pump can substitute with constant pressure funnel or syringe or dropper.
The preferred temperature of heating is 200～500 ℃ in the described high temperature furnace of step (4), and the heating retention time is 30～600 minutes.
Above-mentioned polyalcohol is ethylene glycol, pentanediol, sorbierite, glycerine or pentaerythrite.
Above-mentioned high molecular surfactant is polyvinylpyrrolidone, chloro-hexadecane yl pyridines, hexadecyltrimethylammonium chloride, diallyl dimethyl ammoniumchloride or softex kw.
The salt of above-mentioned silver ion is anhydrous nitric acid silver, silver trifluoromethanesulfonate or silver acetate.
The preferred anhydrous assay polyalcohol of polyalcohol; Polyvinylpyrrolidone is preferably analyzed pure pressed powder, and mean molecule quantity is 10000～100000; Halogen-containing slaine is preferably analyzed pure pressed powder.
The present invention uses halogen-containing slaine assistant, and the metal ion of assistant plays the effect of the growth of reforming as the sacrifice agent of oxygen in the reaction to the silver-colored nucleus that restores; The halide ion of assistant plays the effect of slowly-releasing as the compounding ingredient of silver ion to silver ion in reaction, it is slowly restored; At the following silver nano material that grows size, pattern homogeneous and controllable of inducing jointly of two kinds of effects.
The present invention is divided into three batch processings with raw material, the synthetic of silver nano material is a kind of process of crystal growth, and it is in order effectively to control the coordination between silver ion and the high molecular surfactant that the salting liquid and the high molecular surfactant solution separate configuration of silver ion are mixed again.Under the weak solution state, effectively promote its interionic coordination degree, thereby help adding in the back the formation and the growth of thermal process reactor nucleus.
The present invention compares with the technology that existing solution prepares silver nano material mutually, has the following advantages: the appearance of nano material that (1) obtains is even, the purity height, and monodispersity is good; (2) cost is relatively low, and deinstall is comparatively simple; (3) this method pattern is controlled, the size modification scope is wide, can realize that silver nano material is synthetic on a large scale, has industrial prospect.
Description of drawings
Fig. 1 is nano silver wire SEM (SEM) figure of 70 nanometers for the diameter of preparation in the embodiment of the invention 1.
Fig. 2 is the diameter distribution map of the nano silver wire of 70 nanometers for the diameter of preparation in the embodiment of the invention 1.
Fig. 3 is nano silver wire SEM (SEM) figure of 40 nanometers for the diameter of preparation in the embodiment of the invention 2.
Fig. 4 is nano silver wire SEM (SEM) figure of 120 nanometers for the diameter of preparation in the embodiment of the invention 3.
Fig. 5 is the diameter distribution map of the nano silver wire of 120 nanometers for the diameter of preparation in the embodiment of the invention 3.
Fig. 6 is nano silver wire SEM (SEM) figure of 250 nanometers for the diameter of preparation in the embodiment of the invention 4.
Fig. 7 is the diameter distribution map of the nano silver wire of 250 nanometers for the diameter of preparation in the embodiment of the invention 4.
Fig. 8 is nano silver wire SEM (SEM) figure of 500 nanometers for the diameter of preparation in the embodiment of the invention 5.
Fig. 9 is silver nano-grain SEM (SEM) figure of 50 nanometers for the diameter of preparation in the embodiment of the invention 6.
Figure 10 is silver nano-grain SEM (SEM) figure of 100 nanometers for the diameter of preparation in the embodiment of the invention 7.
Figure 11 is SEM (SEM) figure of the silver nano material for preparing in the Comparative Examples.
The specific embodiment
The embodiment that below provides will the invention will be further described in conjunction with the accompanying drawings.
Embodiment 1:
First preparation ethylene glycol, polyvinylpyrrolidone and copper chloride mixed solution: take by weighing 1 gram polyvinylpyrrolidone join stir in 25 milliliters of ethylene glycol or ultrasonic dissolution after add 6 milligrams of KBrs and 6 milligrams of copper chlorides again, stir or ultrasonic dissolution evenly standby.Prepare ethylene glycol and silver nitrate mixed solution again: take by weighing 1 gram silver nitrate join in 25 milliliters of ethylene glycol stir or the concussion dissolving evenly standby.Get 45 milliliters of ethylene glycol then and join in the reactor, ultrasonic heating is after 30 minutes; Add 2 ml waters again and continued ultrasonic 15 minutes, ethylene glycol mixed solution with the silver nitrate ethylene glycol solution for preparing and polyvinylpyrrolidone and copper chloride injects reactor with the speed of 1 ml/min by syringe pump simultaneously then, after dripping end, seal reactor and place high temperature furnace to heat 120 minutes down for 200 ℃.After reaction stopped, each 50 milliliters of water and ethanol cleaned and are centrifugal, at last the gained precipitation were carried out drying and can obtain the nano silver wire that dry powder shape diameter is 1～20 micron of 70 nanometer, length.Fig. 1 is the nano silver wire scanning electron microscope diagram of diameter 70 nanometers, and products obtained therefrom is the high-purity silver nano wire as seen from Figure 1, is not mingled with any particle.
Embodiment 2:
Similar with the process of embodiment 1, but when the preparation silver nano material, will contain; The halide ion inorganic salts are replaced by potassium chloride by copper chloride, and consumption is reduced to 4 milligrams.The ultrasonic heat hot of ethylene glycol time decreased to 15 minute, other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the nano silver wire that diameter is 40 nanometers.Fig. 3 is the nano silver wire scanning electron microscope diagram of diameter 40 nanometers, and the nano silver wire of diameter 40 nanometers still keeps the axial length of overlength as seen from Figure 3.
Embodiment 3:
Similar with the process of embodiment 1, but when the preparation silver nano material, the rate of addition of syringe pump increases to 1.5 ml/min, is added dropwise to complete heating under 160 degree in high temperature furnace, is reduced to 30 minutes heat time heating time, and other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the nano silver wire that diameter is 120 nanometers.Fig. 4 is the nano silver wire scanning electron microscope diagram of diameter 120 nanometers, and when can find out that by Fig. 4,5 the nano silver wire diameter increases, axial length slightly reduces, but still keeps high-purity and high monodispersity.
Embodiment 4:
Similar with the process of embodiment 1, but when the preparation silver nano material, the ethylene glycol consumption is reduced to 20 milliliters during ultrasonic heating, be reduced to heat time heating time 10 minutes, the syringe pump rate of addition is reduced to 0.75 ml/min, drip the end back and continue to extend to 90 minutes heat time heating time in high temperature furnace, other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the nano silver wire that diameter is 250 nanometers.Fig. 6 is the nano silver wire scanning electron microscope diagram of diameter 250 nanometers, can find out that by Fig. 6,7 nano silver wire has higher draw ratio and high product purity.Because the reaction time is longer, monodispersity descends to some extent.
Embodiment 5:
Similar with the process of embodiment 1, but when the preparation silver nano material, regulating the polyvinylpyrrolidone consumption is 0.5 gram, the silver nitrate consumption is 1.5g, and the syringe pump rate of addition is adjusted to 2 ml/min, and other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the nano silver wire that diameter is 500 nanometers.Fig. 8 is the nano silver wire scanning electron microscope diagram of diameter 500 nanometers.
Embodiment 6:
Similar with the process of embodiment 1, but in preparation during silver nano material, regulating the polyvinylpyrrolidone consumption is 0.5 gram, the silver nitrate consumption is 1.5g, and the syringe pump rate of addition is adjusted to 2 ml/min, and copper chloride becomes copper nitrate, and other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the silver nano-grain that diameter is 50 nanometers.Fig. 9 is the silver nano-grain scanning electron microscope diagram of diameter 50 nanometers.
Embodiment 7:
Similar with the process of embodiment 1, but when the preparation silver nano material, ethylene glycol is replaced by pentanediol; Polyvinylpyrrolidone is replaced by the chloro-hexadecane yl pyridines; Silver nitrate is replaced by silver trifluoromethanesulfonate, and consumption remains unchanged; Halogen-containing ion inorganic salts are replaced by potassium chloride by KBr, and consumption is reduced to 4 milligrams; The cupric inorganic salts are replaced by copper nitrate by copper chloride, and consumption is 6 milligrams.Pentanediol is reduced to 15 minutes ultrasonic heat time heating time, and other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, the sediment low temperature drying to the dry powder shape, can be obtained the silver nano-grain that diameter is 200 nanometers.Figure 10 is the silver nano-grain scanning electron microscope diagram of diameter 200 nanometers.
Comparative Examples:
Similar with the process of embodiment 1, but when the preparation silver nano material, do not add any assistant, other conditions remain unchanged.After reaction finishes, with ethanol, ultra-pure water washing centrifugal after, with the sediment low temperature drying to the dry powder shape, the product pattern heterogeneity that obtains.Figure 11 is the scanning electron microscope diagram of this product.
Claims (10)
1. a method for preparing serial high-purity silver nano material is characterized in that, comprises that step is as follows:
(1) polyalcohol, high molecular surfactant, halogen-containing slaine assistant are stirred or ultrasonic dissolution, get mixed solution A;
(2) salt with polyalcohol and silver ion dissolves through stirring or shaking, and gets mixed solution B;
(3) add an amount of polyalcohol in reactor, adopt ultrasonic mode of heating heating 5～60 minutes, add certain water gaging again, the continuation sonic oscillation also heated 1～30 minute;
(4) mixed solution A and B are added drop-wise in the aforesaid reaction vessel, with the reactor sealing, are positioned over high temperature furnace then and descend and kept 10～1000 minutes for interior 100～600 ℃ after being added dropwise to complete.
2. the method for the serial high-purity silver nano material of preparation according to claim 1, it is characterized in that described halogen-containing slaine assistant is the mixture of one or more and cupric inorganic salts in KBr, zinc chloride, sodium chloride, potassium chloride, iron chloride, sodium bromide, KI, the sodium iodide.
3. the method for the serial high-purity silver nano material of preparation according to claim 2 is characterized in that, described cupric inorganic salts are one or more in copper bromide, copper chloride, copper nitrate, copper sulphate, the copper acetate.
4. the method for the serial high-purity silver nano material of preparation according to claim 2 is characterized in that, described halogen-containing slaine assistant is that KBr mixes with mol ratio with copper chloride at 1: 1.
5. the method for the serial high-purity silver nano material of preparation according to claim 1 is characterized in that, the usage ratio of polyalcohol was 1: 1: 1 during step (1), (2), (3) three went on foot.
6. according to the method for claim 1, the serial high-purity silver nano material of 2 or 3 described preparations, it is characterized in that, the usage ratio of polyalcohol, high molecular surfactant is 5～1000ml: 0.01～50g in the step (1), and high molecular surfactant and halogen-containing slaine assistant mass ratio are 10～50000: 0.05～100.
7. the method for the serial high-purity silver nano material of preparation according to claim 1 is characterized in that, the usage ratio of the salt of polyalcohol and silver ion pass is 5～1000ml in the step (2): 0.01～50g.
8. the method for the serial high-purity silver nano material of preparation according to claim 1 is characterized in that described polyalcohol is ethylene glycol, pentanediol, sorbierite, glycerine or pentaerythrite.
9. the method for the serial high-purity silver nano material of preparation according to claim 1, it is characterized in that described high molecular surfactant is polyvinylpyrrolidone, chloro-hexadecane yl pyridines, hexadecyltrimethylammonium chloride, diallyl dimethyl ammoniumchloride or softex kw.
10. according to the method for claim 1 or the serial high-purity silver nano material of 7 described preparations, it is characterized in that the salt of described silver ion is anhydrous nitric acid silver, silver trifluoromethanesulfonate or silver acetate.
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