CN102303124A - Method for preparing length-diameter-ratio nano-silver wire by pH-value regulation solvothermal method - Google Patents
Method for preparing length-diameter-ratio nano-silver wire by pH-value regulation solvothermal method Download PDFInfo
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Abstract
The invention relates to a method for preparing a length-diameter-ratio nano-silver wire by a pH-value regulation solvothermal method. The method comprises the following steps of: preparing the following ethylene glycol solution, namely an ethylene glycol solution A of silver nitrate or silver acetate, an ethylene glycol solution B of polyvinyl pyrrolidone (PVP), an ethylene glycol solution C of water-soluble chloride and concentrated acid D; mixing the components according to a certain amount and fully stirring to form a final mixed solution; moving the final mixed solution into a reaction kettle; placing in an oven for reaction for a certain time; taking the reaction kettle out and cooling to room temperature to obtain mother liquid of the nano-silver wire; adding alcohol into the mother liquid for diluting, and removing supernatant liquor to obtain a precipitate; and repeatedly performing centrifugal separation, and thus obtaining nano-silver wire dispersion liquid uniformly dispersed in the alcohol. The method is simple, high in efficiency and low in cost, and can prepare high-quality nano-silver wires within a wider range of reaction condition; and prepared products are high in length-diameter ratio, good in length uniformity and low in impurity content.
Description
Technical field
The present invention relates to the nano-silver thread field of material preparation, refer in particular to a kind of method for preparing the high length-diameter ratio nano-silver thread: the solvent-thermal method that the pH value is regulated.
Background technology
Metal nano material is representative as an important branch of nano materials research with noble metal gold, silver, copper, and wherein Nano Silver obtains maximum concerns because of its wide application prospect.Because Nano Silver has very stable physics and chemical property, have very excellent performance at aspects such as electronics, optics, antibiotic and catalysis, can be widely used in catalyst material, battery electrode material, optical material, anti-biotic material, coating etc.For example, Nano Silver has high electric conductivity and thermal conductivity, makes its conductive filler that can be used as conducting resinl, obtaining can to reduce the use amount of conductive filler greatly on the basis of electric conductivity preferably, plays the effect that improves the conducting resinl shear strength.The excellent performance of these of Nano Silver depends primarily on the series of physical parameter, like size, pattern and structure etc.Wherein, obtained more attention, be it and realize control more easily Nano Silver character for the control of Nano Silver pattern.For example, the peak position at surface plasma resonance (SPR) peak and the number pattern that depends primarily on Nano Silver; Red shift can take place along with the increase of the excellent draw ratio of Nano Silver in long axis direction plasma resonance (SPR) pattern of Nano Silver rod.Therefore, the controlled preparation and the application of research Nano Silver have great importance.
Along with the appearance of the flexible and transparent electrode material that is used for alternative ito glass, the material supply section scholar has paid a large amount of effort and has had good electrical conductivity and light transmittance simultaneously to seek a kind of better conductive material.The nano silver wire material becomes the preferred material for preparing the flexible and transparent electrode with the electric conductivity of its superelevation and characteristic such as preparation and receiving much concern easily.Consider that from the light transmittance and the electric conductivity angle of flexible and transparent electrode people hope that more the nano-silver thread of being filled has suitable diameter, high draw ratio is easy to preparation in enormous quantities, and free from admixture.Higher draw ratio helps nano-silver thread and when being overlapped to form conductive network, has node still less, and to reduce these internodal contact resistances, the flexible and transparent electrode that causes the less nano-silver thread of draw ratio to be worked it out has higher side's resistance and low light transmittance.The nano-silver thread that can prepare the draw ratio with suitable diameter and Geng Gao becomes the key technology of preparation transparency electrode, and industrial circle is also strong day by day for the demand with nano-silver thread of high length-diameter ratio more.
At present, the method for synthesizing nano-silver line is a lot, and method commonly used mainly is the polyalcohol method.Xia etc. [1] are crystal seed with Pt or Ag, and having prepared diameter is the nano-silver thread of 30-50nn, and length has reached 50 microns.Yet there is following problem in the polyalcohol method: l) adopt peristaltic pump to drip silver nitrate and PVP solution simultaneously, cost is high, and the dropping time is longer; 2) Nano Silver of preparation different-shape needs to regulate rate of addition; 3) complex process is unfavorable for enlarging and produces.Zaleski etc. [2] combine microwave method with traditional polyalcohol method; Equally also in solution, add a certain amount of sodium chloride; Finally can form the uniform nano-silver thread of size; This makes that adopting the auxiliary polyalcohol method of microwave to prepare the nano silver wire material fast becomes possibility; Chinese patent: (application number is: 200810019828.6), (application number is: 200810163102.X) (application number is: 200910006131.X) (4) a kind of cation control microwave method prepares the method for the controlled nano silver wire in line footpath to the method for (3) a kind of microwave auxiliary preparation of different-shape silver nanostructured material to (2) a kind of method for preparing noble metal nano wire in enormous quantities to the method for (1) preparing silver nano-wire in large batch, and (application number is: 201010559335.9) respectively the auxiliary polyalcohol method legal system of microwave is equipped with the nano-silver thread material and reports; Though that is reported can both prepare the nano silver wire material; Yet prepared nano-silver thread material line length is all shorter, generally speaking all is no more than 30 microns, and draw ratio is all smaller; And containing a large amount of impurity in its nano-silver thread for preparing, length uneven distribution phenomenon is more serious.Zhang [3] and Chen [4] etc. combine traditional polyalcohol method with hydro-thermal method; Introduce a certain amount of sodium chloride and FeCl3 and Na2S, chlorion wherein and sulphion can combine to generate AgCl or Ag2S colloid with silver ion; When colloid concentration was low, it was as the crystal seed that generates nano-silver thread; When colloid concentration was higher, this colloid helped generating the Nano Silver cubic block as inhibitor.Though this method has realized the controlledly synthesis of Nano Silver material; Yet the prepared nano-silver thread draw ratio that gets is not high; Like this when the preparation electrode material; Under the same filling rate situation, the nano-silver thread that draw ratio is low is because the number of nodes nano-silver thread high than draw ratio increases greatly, and its electric conductivity will differ from an one magnitude.
So, how to realize that the nano silver wire material preparation of high length-diameter ratio and the prepared nano-silver thread impurity content that comes out are few, the length good uniformity becomes restriction flexible and transparent electrode material and realizes industrialized one big restraining factors.
Pertinent literature is following:
[1] SunY.; Yin Y.; Mayers B.T.; Et al.Uniform silver nanowires synthesis by redueing AgNO3 with ethylene glycol in the Presence of seeds and Poly (VinylPyrrolidone). Chemistry of Materials, 2002,14 (11): 4,736 1 4745.
[2 " Gou L., Chipara M., Zaleski J.M. Convenient, rapid synthesis of Ag nanowires. Chemistry of Materials, 2007,19 (7): 1,755 1 1760.
[3]?Zhang?W.C.?Wu?X.L.?Chen?H.T.et?al.?Self-organized?formation?of?silver?nanowires，nanocubes?and?bipyramids?via?a?so1othemal?method.?Acta?Materialia，2008，56(11).
[4] Chen D.P.; Qiao X.L.; Et al.. Convenient synthesis of silver nanowires with adjustable diameters via a solvothermal method. Journal of Colloid andInterface Science; 2010,344 (2): 286 1 291.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the high length-diameter ratio nano silver wire; Prepared nano silver wire material not only draw ratio is high; And productive rate is high; Impurity is few, and thickness and length good uniformity have overcome weakness such as impurity that traditional polyalcohol legal system is equipped with complex technical process and microwave method is many, inhomogeneous.On the basis of traditional polyalcohol method, the solvent-thermal method that adopts the pH value to regulate before reaction, only needs to mix each reactant, subsequently mixed solution is placed agitated reactor, and reaction at a certain temperature gets final product.
In order to reach above technique effect, the present invention adopts following technical scheme: said method comprising the steps of:
At first, the following ethylene glycol solution of configuration:
A: silver nitrate or silver acetate ethylene glycol solution;
B: the ethylene glycol solution of polyvinylpyrrolidone (PVP);
C: the ethylene glycol solution of water soluble chloride;
D: concentrated acid;
Ethylene glycol solution B, the ethylene glycol solution C of water soluble chloride, the concentrated acid D of above-mentioned silver nitrate or silver acetate ethylene glycol solution A, polyvinylpyrrolidone (PVP) are fully stirred by a certain amount of mixings back, and formation final mixed solution moves to it in agitated reactor; After placing baking oven reaction certain hour; Agitated reactor is taken out, behind the cool to room temperature, obtain the mother liquor of nano silver wire; In this mother liquor, add alcohol dilution back under the rotating speed of 1500-4000rpm; Remove the upper strata stillness of night, obtain sediment, repeat to obtain being dispersed in the nano-silver thread dispersion liquid in the alcohol after 1-2 centrifugal separation processes.
Through above technical scheme, the beneficial effect that the present invention has is:
1) preparation technology is simple, and efficient is high, and cost is low, in very wide Reaction conditions range, all can prepare high-quality nano silver wire;
2) the product draw ratio for preparing is high, and impurity is few, the length good uniformity;
3) preparation equipment is simple, amplifies to be used for large-scale production easily.
Description of drawings
The high power stereoscan photograph of the nano silver wire material of Fig. 1 embodiment 1 preparation;
The low power stereoscan photograph of the nano silver wire material of Fig. 2 embodiment 1 preparation;
The high power stereoscan photograph of the nano silver wire material of Fig. 3 embodiment 2 preparations;
The low power stereoscan photograph of the nano silver wire material of Fig. 4 embodiment 2 preparations;
Fig. 5: the high power stereoscan photograph of the nano silver wire material of comparative example 1 preparation;
The low power stereoscan photograph of the nano silver wire material of Fig. 6 comparative example 1 preparation;
The XRD of the nano silver wire of Fig. 7 embodiment 1 preparation characterizes.
The nano silver wire diameter that makes among Fig. 8 embodiment 1-10 and the comparative example 1-2, length and draw ratio form.
The specific embodiment
The invention provides a kind of method for preparing the high length-diameter ratio nano silver wire: the pH value is regulated solvent-thermal method, specifically is the silver nitrate of certain volume ratio or silver acetate ethylene glycol solution, the ethylene glycol solution of polyvinylpyrrolidone (PVP), the ethylene glycol solution of water soluble chloride, concentrated acid are mixed the back and fully stir, and forms final mixed solution; It is moved in the agitated reactor; Placing preset temperature is 120-170 ℃ baking oven, behind the reaction certain hour, agitated reactor is taken out; Behind the cool to room temperature; With will obtaining line footpath between 98nm～376nm after its centrifugation, the nano wire of length between 26 microns～72 microns.The prepared nano silver wire material of this method is draw ratio high (greater than 100) not only, and productive rate is high, and impurity is few, and thickness and length good uniformity have overcome weakness such as impurity that traditional polyalcohol legal system is equipped with complex technical process and microwave method is many, inhomogeneous.
The preparation method that a kind of Nano Silver provided by the present invention is filled high heat-conductivity conducting glue can pass through also A component, B component and C component concentrations are confirmed that the mode of recently controlling mol ratio with volume obtains that like this, canonical process of the present invention is following:
At first, dispose the ethylene glycol solution of following concentration:
A: concentration is silver nitrate or the silver acetate ethylene glycol solution of 0.2mol/L;
B: concentration is the ethylene glycol solution of the polyvinylpyrrolidone (PVP) of 0.4mol/L;
C: concentration is: the ethylene glycol solution of the water soluble chloride of 0.01mol/L;
D: concentrated acid;
The A of certain volume ratio, B, C, D solution are mixed the back fully stir, forms final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 120-170 ℃ baking oven, behind the reaction certain hour, with agitated reactor taking-up, cool to room temperature.Obtain the mother liquor of nano silver wire; The upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds the 500-1000 volume under the rotating speed of 1500-4000rpm, obtain sediment; Repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid; The line footpath of gained nano silver wire material is between 80nm～500nm, and its length is between 30 microns～150 microns, and the draw ratio of gained nano-silver thread is greater than 100 simultaneously.
Embodiment 1:
Carry out according to the preparation process: dispose following solution:
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the manganese chloride of 0.01mol/L;
D: red fuming nitric acid (RFNA);
Get the A of 1000 parts by volume, the B of 1000 parts by volume, the C of 25 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 140 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire; The upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 3000rpm, obtain sediment; Repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid; The sem test sample is that sample is sticked on the aluminium base sample stage, and Fig. 1 has provided the nano silver wire high power SEM photo that obtains according to embodiment 1, and the line footpath of nano-silver thread obtains according to Fig. 1 statistics; Fig. 2 has provided the nano silver wire low power SEM photo that obtains according to embodiment 1, and the length of nano-silver thread obtains according to Fig. 2 statistics.As can be seen from Figure 1, the nano silver wire complete form for preparing, average line directly is 120nm, and line length surpasses 40 microns, and draw ratio is greater than 300; Fig. 7 is that the XRD of the nano silver wire of embodiment 1 preparation characterizes, as can beappreciated from fig. 7 the nano silver wire perfect crystalline.
Embodiment 2:
Carry out according to the preparation process: dispose following solution
A: concentration is the silver acetate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 90 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the iron chloride of 0.01mol/L;
D: red fuming nitric acid (RFNA);
Get the A of 500 parts by volume, the B of 800 parts by volume, the C of 20 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 160 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire; The upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 500 volumes under the rotating speed of 3000rpm, obtain sediment; Repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid; The sem test sample is that sample is sticked on the aluminium base sample stage, and Fig. 3 has provided the nano silver wire high power SEM photo that obtains according to embodiment 1, and the line footpath of nano-silver thread obtains according to Fig. 3 statistics; Fig. 4 has provided the nano silver wire low power SEM photo that obtains according to embodiment 1, and the length of nano-silver thread obtains according to Fig. 4 statistics.As can be seen from Figure 3, the nano silver wire complete form for preparing, average line directly is 98nm, and line length surpasses 33 microns, and draw ratio is greater than 330.
Embodiment 3:
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the sodium chloride of 0.01mol/L;
D: concentrated hydrochloric acid;
Get the A of 200 parts by volume, the B of 250 parts by volume, the C of 20 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 130 ℃ baking oven; Behind the reaction 2.5h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 1500rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 184nm, and line length surpasses 53 microns, and draw ratio is greater than 250.
Embodiment 4:
Carry out according to the preparation process: dispose following solution
A: concentration is the silver acetate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the zinc chloride of 0.01mol/L;
D: red fuming nitric acid (RFNA);
Get the A of 500 parts by volume, the B of 500 parts by volume, the C of 20 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 150 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 700 volumes under the rotating speed of 2000rpm, obtain sediment, repeats will obtain being dispersed in the nano-silver thread dispersion liquid in the alcohol after 1-2 centrifugal separation processes.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 150nm, and line length surpasses 26 microns, and draw ratio is greater than 150.
Embodiment 5
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the magnesium chloride of 0.01mol/L;
D: concentrated hydrochloric acid;
Get the A of 500 parts by volume, the B of 500 parts by volume, the C of 10 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 160 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 1500rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 147nm, and line length surpasses 39 microns, and draw ratio is greater than 200.
Embodiment 6
Carry out according to the preparation process: dispose following solution
A: concentration is the silver acetate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the chloro TBuA of 0.01mol/L;
D: red fuming nitric acid (RFNA);
Get the A of 1000 parts by volume, the B of 1500 parts by volume, the C of 10 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 150 ℃ baking oven; Behind the reaction 3h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 3000rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 161nm, and line length surpasses 38 microns, and draw ratio is greater than 200.
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the cetab of 0.01mol/L;
D: concentrated hydrochloric acid;
Get the A of 200 parts by volume, the B of 200 parts by volume, the C of 20 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 150 ℃ baking oven; Behind the reaction 1h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 500 volumes under the rotating speed of 4000rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 376nm, and line length surpasses 61 microns, and draw ratio is greater than 150.
Embodiment 8
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the copper chloride of 0.01mol/L;
D: red fuming nitric acid (RFNA);
Get the A of 400 parts by volume, the B of 800 parts by volume, the C of 5 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 120 ℃ baking oven; Behind the reaction 4h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 800 volumes under the rotating speed of 3500rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 220nm, and line length surpasses 72 microns, and draw ratio is greater than 300.
Embodiment 9
Carry out according to the preparation process: dispose following solution
A: concentration is the silver acetate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the potassium chloride of 0.01mol/L;
D: concentrated hydrochloric acid;
Get the A of 200 parts by volume, the B of 200 parts by volume, the C of 5 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 150 ℃ baking oven; Behind the reaction 1h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 1500rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 248nm, and line length surpasses 51 microns, and draw ratio is greater than 200.
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the manganese chloride of 0.01mol/L;
D: concentrated hydrochloric acid;
Get the A of 5000 parts by volume, the B of 15000 parts by volume, the C of 10 parts by volume, the D solution of 1 parts by volume mix the back and fully stir; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 170 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire, the upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 1500rpm, obtain sediment, repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid.The line footpath of nano-silver thread is obtained by high power SEM photo statistics, and the length of nano-silver thread obtains according to nano silver wire low power SEM photo statistics, the nano silver wire complete form for preparing, and average line directly is 160nm, and line length surpasses 52 microns, and draw ratio is greater than 300.
The used concentrated hydrochloric acid of the present invention is that commercially available mass concentration is the 37.5%HCl aqueous solution, and red fuming nitric acid (RFNA) is that commercially available mass fraction is 65% the HNO3 aqueous solution.
Comparative example 1:
Carry out according to the preparation process: dispose following solution
A: concentration is the silver nitrate ethylene glycol solution of 0.2mol/L;
B: concentration is that the K value of 0.4mol/L is the ethylene glycol solution of 30 polyvinylpyrrolidone;
C: concentration is: the ethylene glycol solution of the manganese chloride of 0.01mol/L;
Get the A of 1000 parts by volume, the B of 1000 parts by volume, the C of 25 parts by volume mixes the back and fully stirs; Form final mixed solution, mixed solution is moved in the agitated reactor, placing preset temperature is 140 ℃ baking oven; Behind the reaction 2h, agitated reactor is taken out cool to room temperature.Obtain the mother liquor of nano silver wire; The upper strata stillness of night is removed in the alcohol dilution back that in this mother liquor, adds 1000 volumes under the rotating speed of 3000rpm, obtain sediment; Repeat will evenly to be disperseed after 1-2 centrifugal separation processes with alcohol in the nano-silver thread dispersion liquid; The sem test sample is that sample is sticked on the aluminium base sample stage, and Fig. 5 has provided the nano silver wire high power SEM photo that obtains according to comparative example 1, and the line footpath of nano-silver thread obtains according to Fig. 5 statistics; Fig. 6 has provided the nano silver wire low power SEM photo that obtains according to comparative example 1, and the length of nano-silver thread obtains according to Fig. 6 statistics.As can be seen from Figure 5, the nano silver wire complete form for preparing, this nano-silver thread average line directly is 110nm, line length surpasses 10 microns, draw ratio about 90.
Comparative example 2 is the disclosed microwave method preparation of 201010559335.9 Chinese patent according to application number::
Preparing process according to microwave method carries out: (1) joins the silver acetate of 0.1mol in the 500ml ethylene glycol; Prepare argentiferous ion solution reaction system; Be that the polyvinylpyrrolidone of 30 0.5mol joins in this solution system with the K value again, prepare argentiferous ion solution system; (2) the MnCl2 powder with 0.5mmol joins in the 20ml ethylene glycol, stirs, and obtains the settled solution system; (3) in the prepared solution of step (1), drip the ethylene glycol solution of the 20mlMnCl2 that step (2) makes; (4) method of employing microwave irradiation; This precursor that obtains irradiation 14min under the 480W microwave is obtained the nano silver wire material of high length-diameter ratio; The solution of gained behind the microwave irradiation is centrifugal through water or alcohol, washing obtains its uniform dispersion liquid, the nano silver wire complete form for preparing, and average line directly is 128nm; 7 microns of line lengths, draw ratio is less than being 60.
For reaching illustration purpose; This patent is narrated as above with preferred embodiments, and so it is not in order to qualification the present invention, and any affiliated technical field is not breaking away from the spirit and scope of the present invention; When can doing a little change and polishing, so protection scope of the present invention is when exceeding with claims.
Claims (9)
1. the solvent-thermal method of a pH value adjusting prepares the method for high length-diameter ratio nano-silver thread, said method comprising the steps of:
At first, the following ethylene glycol solution of configuration:
A: silver nitrate or silver acetate ethylene glycol solution;
B: the ethylene glycol solution of polyvinylpyrrolidone (PVP);
C: the ethylene glycol solution of water soluble chloride;
D: concentrated acid;
Ethylene glycol solution B, the ethylene glycol solution C of water soluble chloride, the concentrated acid D of above-mentioned silver nitrate or silver acetate ethylene glycol solution A, polyvinylpyrrolidone (PVP) are fully stirred by a certain amount of mixings back, and formation final mixed solution moves to it in agitated reactor; After placing baking oven reaction certain hour; Agitated reactor is taken out, behind the cool to room temperature, obtain the mother liquor of nano silver wire; In this mother liquor, add alcohol dilution back under the rotating speed of 1500-4000rpm; Remove the upper strata stillness of night, obtain sediment, repeat to obtain being dispersed in the nano-silver thread dispersion liquid in the alcohol after 1-2 centrifugal separation processes.
2. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread, it is characterized in that said silver nitrate or silver acetate are that commercially available purity is at the technical grade powder more than 98%.
3. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread, it is characterized in that the K value of said polyvinylpyrrolidone (PVP) is more than 30 or 30.
4. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread; It is characterized in that said water soluble chloride comprises sodium chloride, manganese chloride, iron chloride, potassium chloride, magnesium chloride, zinc chloride, cetab (CTAB), chloro TBuA (TBAC), copper chloride.
5. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread, it is characterized in that said concentrated acid comprises concentrated hydrochloric acid and red fuming nitric acid (RFNA).
6. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread, it is characterized in that the mol ratio of solute is (40 ~ 1000) in said A, B, C, the D solution: (80 ~ 6000): (0.1 ~ 0.25): 1.
7. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread; It is characterized in that; The line footpath of the nano silver wire material that obtains is between 98nm～376nm; Its length is between 26 microns～72 microns, and the draw ratio of gained nano-silver thread is greater than 100 simultaneously.
8. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread, it is characterized in that said baking oven preset temperature is 120-170 ℃.
9. the solvent-thermal method of regulating according to the described a kind of pH value of claim 1 prepares the method for high length-diameter ratio nano-silver thread; It is characterized in that the mol ratio of solute is (500 ~ 1000) in said alcohol and said A, B, C, the D solution: (40 ~ 1000): (80 ~ 6000): (0.1 ~ 0.25): 1.
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| CN201210201644.8A CN102744417B (en) | 2011-06-16 | 2012-06-15 | A kind of preparation method of nano silver wires with high length-diameter ratio |
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