CN104942302A - Preparing method for silver nano-wire with adjustable diameter - Google Patents
Preparing method for silver nano-wire with adjustable diameter Download PDFInfo
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Abstract
The invention discloses a preparing method for a silver nano-wire with an adjustable diameter. The method controls the diameter of the silver nano-wire by adjusting the mixture PVP concentration. The auxiliary salt polyhydric alcohol method is adopted, two or more PVP polyhydric alcohol solutions with different molecular weights are mixed, under the condition of different mixing ratios and different PVP concentrations, and by means of the thermal recovery method of polyhydric alcohol, the silver nano-wire which is controllable in diameter and good in uniformity is prepared. By adjusting parameters, the silver nano-wire is obtained, wherein the average diameter of the silver nano-wire ranges from 30 nm to 300 nm, and the average length of the silver nano-wire ranges from 10 micrometers to 60 micrometers. The preparing method is simple, and easy to operate. The silver nano-wire is controllable in diameter, and good in uniformity. The preparing method is suitable for producing silver nano-wires with specific diameters in a large-scaled mode.
Description
Technical field
The invention belongs to nano material synthesis technical field, be specifically related to a kind of synthetic method rapidly and efficiently of nano silver wire of controlled diameter.
Background technology
Nano silver wire, owing to having the characteristics such as excellent conduction, printing opacity and flex endurant, is therefore regarded as the material most possibly substituting tin indium oxide (ITO).But the controlledly synthesis of the nano silver wire that controlled diameter, homogeneity are good is all the major obstacle that it is applied all the time.Therefore, the synthesis of the nano silver wire of controlled diameter has attracted the concern of numerous scholar.In actual applications in order to improve nano silver wire at photoelectric device as the application performance in organic solar batteries, touch-screen, display particularly flexible electronic device of new generation, the diameter of nano silver wire and draw ratio often need effectively to control.In the silver nano material of the various different-shape of controlledly synthesis and size, people make great progress, and as spherical silver nano particle, silver nanoparticle triangle, nano silver wire and silver nanocubes etc. are all controllably synthesized.Wherein, the synthetic method of nano silver wire is more, but process mostly more loaded down with trivial details, diameter is restive and homogeneity is poor.
In prepared by nano silver wire, (1. Sun, the Yugang such as Xia Younan; Mayers, Brian; Herricks, Thurston; Xia, Younan Nano Lett.2003,3,955. 2. Sun, Yugang; Gates, Byron; Mayers, Brian; Xia, Younan Nano Lett.2002,2,165) it is the method be most widely used at present that the polyol reduction method proposed prepares nano silver wire.The method is the derivant of application salt compounds as silver nanowire growth, obtains nano silver wire by heating polyol process.In addition, the PVP of people's different molecular weight such as Zhang Tong has synthesized silver nanoparticle spheric granules and the nano silver wire of different-shape.But the diameter of its nano silver wire all at about 100nm and its homogeneity need to be improved further.In Chinese patent, if the patent No. is a kind of method that CN104174869A discloses overlength and prepares nano silver wire, but the longer and homogeneity of its preparation process has much room for improvement.Chinese patent CN104289723A provides a kind of method utilizing mixing PVP to prepare minor diameter nano silver wire.Mixed by a certain percentage by PVP molecular weight being respectively 5.5 ten thousand and 1,300,000 and can prepare the nano silver wire of diameter at about 30nm.But gained nano silver wire diameter is not of uniform size, homogeneity needs to be improved further.In addition, to show its nano silver wire diameter adjustable extent less for its SEM picture.Therefore, the above-mentioned preparation method about nano silver wire or temperature higher, or reaction time long especially gained nano silver wire diameter restive.Therefore, seek a kind of simple, wire diameter is controlled and the synthetic method of the good nano silver wire of homogeneity is still a challenge at present.Polyvinylpyrrolidone (PVP) Collaborative Control that the present invention intends choosing two kinds and two or more different molecular weight synthesizes and has special diameter and the good nano silver wire of homogeneity.The present invention is that the synthesis of different-diameter nano silver wire provides a kind of simple, fast tunable and the good synthetic method of homogeneity, and the method once can reach the output of more than 10g, is conducive to large-scale production and application.
Summary of the invention
The technical problem that the present invention solves is the preparation method fast and efficiently of the nano silver wire providing a kind of diameter adjustable, the nano silver wire prepared by the method has good homogeneity and specific diameter, and especially its building-up process is simple, fast and be conducive to implementing suitability for industrialized production.
Technical scheme of the present invention is: the preparation method fast and efficiently of the nano silver wire that a kind of diameter is adjustable utilizes the PVP mixed solution of two kinds and two or more different molecular weight to regulate and control the method for nano silver wire diameter, specifically comprises the following steps:
Steps A: adopt salt auxiliary polyhydric alcohol thermal reduction to prepare the good and nano silver wire of controlled diameter of homogeneity: use polyvalent alcohol as solvent, be dissolved in polyalcohol by a certain amount of salt and complex thereof, stir, concentration is 1 × 10
-5mo/L is to 1 × 10
-2between mo/L, this salting liquid is as the derivant of silver nanowire growth;
Step B: adopt the polyhydric alcohol solutions of the PVP of mixing two kinds and two or more different molecular weights to control the diameter of nano silver wire: the solution of the polyalcohol of preparation mixing PVP, the PVP getting different molecular weight respectively at room temperature stirs and is dissolved in polyalcohol, forms the polyhydric alcohol solutions of mixing PVP of homogeneous different PVP proportionings, variable concentrations;
Step C: by polyalcohol thermal reduction by AgNO
3or CH
3cOOAg is reduced into nano silver wire: take a certain amount of AgNO
3or CH
3in the polyhydric alcohol solutions of the mixing PVP of COOAg ultrasonic dissolution in step B, concentration is 0.0001g/mL to 0.3g/mL;
Step D: the preparation of controlled diameter nano silver wire: pour in the round-bottomed flask of certain volume after being mixed by the solution of step C and step B, add the derivant of steps A preparation, after stirring, round-bottomed flask is put into heating jacket intensification heating, temperature controls 120
dEG Cbetween – 185 DEG C, temperature retention time is 15min – 3h, can obtain better homogeneity and have the nano silver wire of different-diameter.
Described salt in steps A and complex thereof comprise eight water zirconium oxychloride (ZrOCl
2.8H
2o), potassium chloride (KCl), magnesium chloride (MgCl
2), copper chloride (CuCl
2), sodium chloride (NaCl), calcium chloride (CaCl
2), silver chlorate (AgCl), frerrous chloride (FeCl
2), platinous chloride (PtCl
2), Copper dichloride dihydrate (CuCl
22H
2o), cobalt chloride hexahydrate (CoCl
26H
2o), four chloride hydrate gold (AuCl
2.HCl.4H
2o), copper bromide (CuBr
2), KBr (KBr), magnesium bromide (MgBr
2), calcium bromide (CaBr
2), sodium bromide (NaBr), silver bromide (AgBr), chloroplatinic acid hexahydrate (Cl
6h
14o6Pt), softex kw (C
19h
42etc. BrN) one or more in.
Described salt in steps A and complex thereof can be all one or more mixtures, and wherein the concentration of each salt or its complex is 1 × 10
-5mo/L is to 1 × 10
-2between mo/L.
The kind mixing PVP in the polyhydric alcohol solutions of PVP in step B comprises all different types of PVP of molecular weight from 0.35 ten thousand to 176 ten thousand, specifically comprise PVPK12 (0.35 ten thousand), PVPK17 (1.01 ten thousand), PVPK25 (3.2 ten thousand), PVPK30 (4.0 ten thousand), PVPK45 (150,000), PVPK60 (210,000), PVPK70 (400,000), PVPK80 (580,000), PVPK85 (600,000), PVPK90 (630,000), PVPK100 (780,000), PVPK110 (1,100,000), PVPK120 (1,390,000), the mixture of two or more the different molecular weight PVP in PVPK150 (1,760,000).
The percent mass ratio mixing often kind of PVP in the ethylene glycol solution of PVP in step B can from any one quality ratio between 0.01 to 0.99%.
The concentration mixing PVP in step B is 0.001g/mL-0.03g/mL.
Polyalcohol in steps A comprises ethylene glycol, propane diols, glycerine.
In step D, the preparation temperature of nano silver wire controls between 120 DEG C-185 DEG C, and temperature retention time is 15min – 3h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Accompanying drawing explanation
Average diameter 30nm prepared by Fig. 1 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Average diameter 50nm prepared by Fig. 2 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Average diameter 70nm prepared by Fig. 3 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Average diameter 100nm prepared by Fig. 4 the present invention, the stereoscan photograph of the nano silver wire of average line length 60 μm.
Average diameter 150nm prepared by Fig. 5 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Average diameter 200nm prepared by Fig. 6 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Average diameter 300nm prepared by Fig. 7 the present invention, the stereoscan photograph of the nano silver wire of average line length 20 μm.
Specific embodiments
In order to explain the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Its embodiment is:
Step one
Get a certain amount of polyvinylpyrrolidone (PVP), silver nitrate presoma is dissolved in ethylene glycol, obtain mixing homogeneous solution, PVP is selected from PVPK12 (0.35 ten thousand), PVPK17 (1.01 ten thousand), PVPK25 (3.2 ten thousand), PVPK30 (4.0 ten thousand), PVPK45 (150,000), PVPK60 (210,000), PVPK70 (400,000), PVPK80 (580,000), PVPK85 (600,000), PVPK90 (630,000), PVPK100 (780,000), PVPK110 (1,100,000), PVPK120 (1,390,000), two or more different molecular weight PVP in PVPK150 (1,760,000), in described mixed solution, the percent mass ratio of often kind of PVP can from any one quality ratio between 0.01% to 0.99%, and the concentration of mixing PVP is 0.001g/mL to 0.03g/mL, the concentration of silver nitrate is 0.0001g/mL to 0.3g/mL.
Step 2
The mixed solution of step one being joined is transferred in round-bottomed flask, and adding concentration is wherein 1 × 10
-5mo/L is to 1 × 10
-2ethylene glycol solution 10 μ L to the 10mL of the salt between mo/L and complex thereof, stir, this salting liquid is as the derivant of silver nanowire growth; After stirring at room temperature is even, mixed solution is heated to 120 DEG C – 185 DEG C, continues insulation reaction 15min to 3h; Reaction terminates to carry out eccentric cleaning to reactant afterwards, obtains the nano silver wire of special diameter.
The preparation method of the nano silver wire that a kind of diameter of the present invention is adjustable, described salt and complex thereof are selected from eight water zirconium oxychloride (ZrOCl
2.8H
2o), potassium chloride (KCl), magnesium chloride (MgCl
2), copper chloride (CuCl
2), sodium chloride (NaCl), calcium chloride (CaCl
2), silver chlorate (AgCl), frerrous chloride (FeCl
2), platinous chloride (PtCl
2), Copper dichloride dihydrate (CuCl
22H
2o), cobalt chloride hexahydrate (CoCl
26H
2o), four chloride hydrate gold (AuCl
2.HCl.4H
2o), copper bromide (CuBr
2), KBr (KBr), magnesium bromide (MgBr
2), calcium bromide (CaBr
2), sodium bromide (NaBr), silver bromide (AgBr), chloroplatinic acid hexahydrate (Cl
6h
14o6Pt), softex kw (C
19h
42etc. BrN) one or more in.
Embodiment 1
(1) preparation of the ethylene glycol solution of salt and complex thereof: get 0.002g copper chloride (CuCl
2) be dissolved in 10mL ethylene glycol (EG), stir, this salting liquid is as the derivant of silver nanowire growth.
(2) preparation of the ethylene glycol solution of PVP is mixed: take 0.1142g PVPK12 (0.35 ten thousand) and 0.8858g PVPK150 (1,760,000) and be dissolved in 200mL ethylene glycol, dissolve in stirring at room temperature.
(3) preparation of PVP and silver nitrate mixed solution: take 0.4892g silver nitrate and add ultrasonic dissolution in (2), continue to be uniformly mixed the mixed solution A obtaining PVP and silver-colored presoma.
(4) derivant of the silver nanowire growth (1) prepared adds in the mixed solution of A, and stirring at room temperature is even, obtains mixed solution B; B solution to be transferred in round-bottomed flask and in heating jacket, to be warmed up to 145 DEG C, insulation reaction 1h, average diameter can be obtained in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 2
On the basis of embodiment 1, only step (2) need be changed into: take 0.1142g PVPK12 (0.35 ten thousand), 0.3542g PVPK90 (630,000) and 0.5316g PVPK150 (1,760,000) and be dissolved in 200mL ethylene glycol, dissolve in stirring at room temperature.All the other steps are carried out according to embodiment 1, and in 160 DEG C, insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 3
On the basis of embodiment 2, only step (2) need be changed into: take 0.2142g PVPK12 (0.35 ten thousand), 0.3542g PVPK90 (630,000) and 0.4316g PVPK150 (1,760,000) and be dissolved in 200mL ethylene glycol, dissolve in stirring at room temperature.All the other steps are carried out according to embodiment 1, in 170 DEG C of insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 4
On the basis of embodiment 2, only step (1) need be changed into: get 0.008g chloroplatinic acid hexahydrate (Cl
6h
14o6Pt) be dissolved in 10mL ethylene glycol (EG), stir, this salting liquid is as the derivant of silver nanowire growth.All the other steps are carried out according to embodiment 1, in 145 DEG C of insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 5
On the basis of embodiment 3, only step (3) need be changed into: take 0.7892g silver nitrate and add ultrasonic dissolution in (2), continue to be uniformly mixed the mixed solution A obtaining PVP and silver-colored presoma.All the other steps are carried out according to embodiment 1, in 145 DEG C of insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 6
On the basis of embodiment 2, only step (1) need be changed into: get 0.008g tetra-chloride hydrate gold (AuCl
2.HCl.4H
2o) be dissolved in 10mL ethylene glycol (EG), stir, this salting liquid is as the derivant of silver nanowire growth.All the other steps are carried out according to embodiment 2, in 160 DEG C of insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Embodiment 7
On the basis of embodiment 6, only step (3) need be changed into: take 0.9892g silver nitrate and add ultrasonic dissolution in (2), continue to be uniformly mixed the mixed solution A obtaining PVP and silver-colored presoma.All the other steps are carried out according to embodiment 6, in 145 DEG C of insulation reaction 1h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
Claims (8)
1. a preparation method for the nano silver wire that diameter is adjustable, is characterized in that: utilize the PVP mixed solution of two kinds and two or more different molecular weight to regulate and control the method for nano silver wire diameter, specifically comprise the following steps:
Steps A: adopt salt auxiliary polyhydric alcohol thermal reduction to prepare the good and nano silver wire of controlled diameter of homogeneity: use polyvalent alcohol as solvent, be dissolved in polyalcohol by a certain amount of salt and complex thereof, stir, concentration is 1 × 10
-5mo/L is to 1 × 10
-2between mo/L, this salting liquid is as the derivant of silver nanowire growth;
Step B: adopt the polyhydric alcohol solutions of the PVP of mixing two kinds and two or more different molecular weights to control the diameter of nano silver wire: the solution of the polyalcohol of preparation mixing PVP, the PVP getting different molecular weight respectively at room temperature stirs and is dissolved in polyalcohol, forms the polyhydric alcohol solutions of mixing PVP of homogeneous different PVP proportionings, variable concentrations;
Step C: by polyalcohol thermal reduction by AgNO
3or CH
3cOOAg is reduced into nano silver wire: take a certain amount of AgNO
3or CH
3in the polyhydric alcohol solutions of the mixing PVP of COOAg ultrasonic dissolution in step B, concentration is 0.0001g/mL to 0.3g/mL;
Step D: the preparation of controlled diameter nano silver wire: pour in the round-bottomed flask of certain volume after the solution of step C and step B is mixed, add the derivant of steps A preparation, after stirring, round-bottomed flask is put into heating jacket intensification heating, temperature controls between 120 DEG C – 185 DEG C, temperature retention time is 15min – 3h, can obtain better homogeneity and have the nano silver wire of different-diameter.
2. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, is characterized in that: the described salt in steps A and complex thereof comprise eight water zirconium oxychloride (ZrOCl
2.8H
2o), potassium chloride (KCl), magnesium chloride (MgCl
2), copper chloride (CuCl
2), sodium chloride (NaCl), calcium chloride (CaCl
2), silver chlorate (AgCl), frerrous chloride (FeCl
2), platinous chloride (PtCl
2), Copper dichloride dihydrate (CuCl
22H
2o), cobalt chloride hexahydrate (CoCl
26H
2o), four chloride hydrate gold (AuCl
2.HCl.4H
2o), copper bromide (CuBr
2), KBr (KBr), magnesium bromide (MgBr
2), calcium bromide (CaBr
2), sodium bromide (NaBr), silver bromide (AgBr), chloroplatinic acid hexahydrate (Cl
6h
14o6Pt), softex kw (C
19h
42etc. BrN) one or more in.
3. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, is characterized in that: the described salt in steps A and complex thereof can be all one or more mixtures, and wherein the concentration of each salt or its complex is 1 × 10
-5mo/L is to 1 × 10
-2between mo/L.
4. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, it is characterized in that: the kind mixing PVP in the polyhydric alcohol solutions of PVP in step B comprises all different types of PVP of molecular weight from 0.35 ten thousand to 176 ten thousand, specifically comprise PVPK12 (0.35 ten thousand), PVPK17 (1.01 ten thousand), PVPK25 (3.2 ten thousand), PVPK30 (4.0 ten thousand), PVPK45 (150,000), PVPK60 (210,000), PVPK70 (400,000), PVPK80 (580,000), PVPK85 (600,000), PVPK90 (630,000), PVPK100 (780,000), PVPK110 (1,100,000), PVPK120 (1,390,000), the mixture of two or more the different molecular weight PVP in PVPK150 (1,760,000).
5. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, is characterized in that: the percent mass ratio mixing often kind of PVP in the ethylene glycol solution of PVP in step B can from any one quality ratio between 0.01 to 0.99%.
6. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, is characterized in that: the concentration mixing PVP in step B is 0.001g/mL-0.03g/mL.
7. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, is characterized in that: the polyalcohol in steps A comprises ethylene glycol, propane diols, glycerine.
8. the preparation method of the nano silver wire that a kind of diameter according to claim 1 is adjustable, it is characterized in that: in step D, the preparation temperature of nano silver wire controls between 120 DEG C-185 DEG C, temperature retention time is 15min – 3h, can obtain average diameter in 30nm – 300nm, average length at the nano silver wire of 10 – 60 μm.
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