CN102699341B - A kind of wet chemical preparation method of silver-colored micro-/ nano line - Google Patents
A kind of wet chemical preparation method of silver-colored micro-/ nano line Download PDFInfo
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- CN102699341B CN102699341B CN201210127527.1A CN201210127527A CN102699341B CN 102699341 B CN102699341 B CN 102699341B CN 201210127527 A CN201210127527 A CN 201210127527A CN 102699341 B CN102699341 B CN 102699341B
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Abstract
The present invention relates to a kind of preparation method of silver-colored micro-/ nano line, described method is under cryogenic, is added by template in silver salt solution, then instills reducing agent wherein, after dropwising, obtains silver-colored micro-/ nano line through washing, drying.The operating temperature of the method for the invention is low, does not add any macromolecule dispersant, carries out completely in an aqueous medium, simple to operate, easily control, reaction environmental protection, low cost.
Description
Technical field
The present invention relates to a kind of wet chemical preparation method of silver-colored micro-/ nano line, belong to inorganic nanowire material field.
Background technology
Metal nanoparticle has high surface energy relative to block materials, special optical property, macroscopic property, physics and chemistry character, and especially the synthesis of anisotropy noble metal has become the focus of Recent study.Metal nanoparticle all plays very important effect in many different fields and becomes study hotspot, as the system that supplies a model for the impact of experimental detection quantum confinement effect on electrical, magnetic and other correlated performances; Also be widely used in the fields such as photodevelopment, catalysis, biomarker, photonic propulsion, photoelectronics, information storage and surface enhanced effect simultaneously.Its character of the size of metal nanoparticle, shape, composition, degree of crystallinity and structures shape.
One-dimensional micro-nanometer structural material, as the micro-nano rice noodles of noble metal Au, Ag and some other oxide, nitride, nanometer rods and nanotube, due to the electricity of its uniqueness, optics, magnetics and thermal property, it is made on microelectronic component, opto-electronic device, sensor, to have boundless application prospect and receive much concern.Explore the focus that preparation low-dimensional micro Nano material that is structurally ordered, function admirable is research always, Ag micro-nano rice noodles are also more and more subject to people's attention, and main cause is that, in all metals, Ag shows extraordinary conduction and heat conductivility.
The preparation method of Ag nanometer rods and/or nano wire is also many, is substantially divided into 3 kinds, hard template method, soft template method and wet chemistry method.
Hard template method utilizes anodic oxidation Woelm Alumina, DNA molecular chain, CNT etc. for template, and deposition has the Nano silver grain of certain pore size size.Such as utilize DNA network, nano-pore Al
2o
3, flat AgBr crystal, the physical template such as mesoporous MCM-41 prepare Ag nano wire etc.The number of nanowires that hard template method is prepared at every turn is limited, nano wire and template separation difficulty, and easily damages in separation process.
Soft template method is the rod-shaped micelle that utilizes surfactant etc. to be formed for the growth of one dimension Nano silver grain provides space.Such as under surfactant polyvinylpyrrolidone (PVP) existent condition, using Pt nano particle as seed, with vinyl hexylene glycol reduction AgNO
3solution, obtains diameter 30-40nm at 160 DEG C, and length-controllable reaches the nano silver wire of 50 μm; Or by UV photoreduction AgNO
3solution synthesizes silver-colored line nano particle, and the nano silver wire diameter obtained is 20-30nm, long 2.5 μm.
The generalized definition of wet chemistry method is have that liquid phase is participated in, prepared material by chemical reaction method; Narrow sense says that coprecipitation is wet chemistry method.Electrochemical deposition method and hydro-thermal reaction all can be regarded as the category of wet chemistry method.Electrochemical deposition method silver electrode is constantly distributed in liquid phase by arc discharge heat release, forms ag nano-cluster.Such as by solid-liquid phase arc discharge method (SLPAD), making the NaNO of electrode with silver
3generate the colloidal solution including Ag cluster in solution, along with the prolongation of ageing time, nano silver wire grows gradually.Hydro-thermal reaction is that what to complete in closed container is chemical method, under making water be in HTHP (being greater than critical point), improves the solubility of solid, the reaction between accelerating solid.
CN02159098.2 discloses a kind of DMF that adopts and prepares the method for nano silver wire at butyl titanate and acetylacetone,2,4-pentanedione as medium as reducing agent.First by butyl titanate and acetylacetone,2,4-pentanedione by volume 1: proceed to again in cucurbit after (0.2-5) ratio mixes; Then by AgNO
3the aqueous solution mixes with the pure DMF of analysis (DMF), wherein AgNO
3in DMF, concentration range is 10
-4-0.1g/ml, adds after being mixed evenly in cucurbit, constantly stirs simultaneously; Mixed liquid carries out reaction 2-24 hour at 50-70 DEG C, and centrifugation obtains nano silver wire.
CN200810019828.6 discloses a kind of ethylene glycol that adopts as reducing agent, and PVP, as protective agent, reduces the method for silver nitrate, preparing silver nano-wire in large batch under the condition of heating using microwave.Described method selection concentration is the anhydrous nitric acid silver AgNO of 99.9%
3, concentration be 99.8% without water glycol C
2h
6o
2, concentration is the polyvinylpyrrolidone PVP molecular weight 55000 of 98% is raw material, in the environment of microwave radiation technology, adopts the method for reduction of ethylene glycol silver nitrate to prepare nano silver wire in large quantity.
It is template that CN201110200278.X discloses the anodised multiaperture pellumina of a kind of employing, and in its hole, utilize the way deposition of chemical deposition to fill silver bromide, the decomposition under ultraviolet light of recycling silver bromide, removing template obtains the method for nano silver wire.
The preparation method of the nano silver wires such as soft template method, hard template method, electrochemical deposition method, control procedure is complicated, and reaction temperature is high, and the reaction time is long.
Caswell etc. have reported for work a kind of surfactant or polymer of not needing as the directed agents of nanowire growth, also do not need the simple wet chemical synthesis of other shape derivants.The method is under 100 DEG C of conditions, in NaOH solution, with citric acid reduction AgNO
3obtained metal A g, obtaining average diameter is 35nm, the nano-silver thread that length is 12 μm.(Surfactantless Wet Chemical Synthesis of SilverNanowires [J]., Caswell, K.K., Bender, C.M., Murphy, C.J.Seedless, NANOLETTERS, 2003,3 (5): 667-669.) method of reporting for work such as Caswell, reaction temperature high (at least wanting 100 DEG C), meanwhile, the form of addition to product of NaOH solution has very big-difference, reaction is responsive, inconvenient operation.
The preparation method of existing nano silver wire, there is course of reaction complexity, inconvenient operation, reaction temperature is high, at least wants 100 DEG C just can carry out.Therefore, how to develop a kind of reaction temperature lower, preparation technology is simple, and operating again the preparation method of silver-colored micro-/ nano line easily, is a problem demanding prompt solution.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the preparation method providing a kind of silver-colored micro-/ nano line.The preparation method of silver-colored micro-/ nano line of the present invention is wet chemical preparation method, and particularly, described method is under cryogenic, template is added in silver salt solution, then instill reducing agent wherein, after dropwising, obtain silver-colored micro-/ nano line through washing, drying.
The present invention carries out in an aqueous medium, does not add any macromolecule dispersant, under doing the condition of template, adopts at a lower temperature at the compound containing citrate ion, and reduction silver nitrate prepares the method for silver-colored micro-/ nano line.Low temperature of the present invention is less than 60 DEG C.
Nano wire is a kind of nanoscale (1 nanometer=10
-9rice) line, change a kind of saying, nano wire can be defined as one and have the one-dimentional structure being limited in below 100 nanometers (longitudinally do not limit) in the horizontal.Micro-/ nano line of the present invention refers to have and is limited in less than 50 microns in the horizontal, the one-dimentional structure that diameter is less than 1 micron.
The preparation method of silver-colored micro-/ nano line of the present invention is under template existent condition, and by reducing agent, silver salt solution reduction is obtained silver-colored micro-/ nano line, described reducing agent is ferrous salt, and described template is the compound containing citrate ion.
Reaction principle of the present invention is as follows: the complexing utilizing citrate, first the complex compound of silver salt and citrate is generated with silver salt complexing, then there is reduction and be obtained by reacting silver-colored micro-/ nano particle in this complex compound under the effect of reducing agent, with the seed that the silver-colored micro-/ nano particle obtained is grow nanowire, under the continued reduction of reducing agent, the complex compound of silver salt and citric acid continues to be reduced, and theoretical by Ostwald slaking, the silver-colored micro-/ nano line of final generation.
The compound of the present invention to citrate ion does not have concrete restriction, and any one can be selected can to provide the material of citrate.In the compound of citrate ion, the counter ion counterionsl gegenions of citrate can be selected from the combination of any a kind or at least 2 kinds in alkali metal ion, alkaline-earth metal ions and transition metal ions, such as Na
+, K
+, Mg
2+, Fe
3+, Al
3+in the combination of any a kind or at least 2 kinds, the ion of described combination is as Na
+/ K
+, i.e. potassium citrate sodium.Citric acid itself has three hydrogen atoms, and in the compound of citrate ion, counter ion counterionsl gegenions can replace 1 hydrogen, 2 hydrogen or 3 hydrogen.The example replacing 1 hydrogen has natrium citricum, potassium citrate etc.; The example replacing 2 hydrogen has disodium citrate, citric acid dipotassium, potassium citrate sodium etc.; The example replacing 3 hydrogen has trisodium citrate, citric acid tri potassium etc.The professional knowledge that those skilled in the art can grasp according to oneself or consult the compound of pertinent literature to citrate ion and select.
Preferably, the compound of citrate ion of the present invention is selected from 1 in citric acid, trisodium citrate, disodium citrate, natrium citricum, potassium citrate, potassium citrate sodium, citric acid dipotassium and citric acid tri potassium or the combination of at least 2 kinds, described combination is natrium citricum/potassium citrate, natrium citricum/citric acid/disodium citrate, citric acid/potassium citrate/citric acid dipotassium/citric acid tri potassium etc. such as, 1 kind in optimization citric acid, natrium citricum and potassium citrate or the combination of at least 2 kinds, further optimization citric acid.
Reducing agent of the present invention is ferrous salt.Fe
2+be ferrous ion, his salt is just ferrous salt.Ferrous salt can be oxidized to Fe
3+, can Fe be reduced to again.The present invention utilizes the reproducibility of ferrous salt, and silver salt is reduced into elemental silver.
The present invention does not have special restriction to the selection of ferrous salt yet, and any one can be selected can to provide ferrous compound.In ferrous salt, the counter ion counterionsl gegenions of ferrous ion are selected from sulfate radical, nitrate anion etc., the principle of selection be ferrous salt must water-soluble and counter-ion can not with silver ion generation chemical reaction.The professional knowledge that those skilled in the art can grasp according to oneself or consult pertinent literature ferrous salt is selected.
Preferably, ferrous salt of the present invention is selected from the combination of in ferrous sulfate, ferrous nitrate a kind or at least 2 kinds, and described combination is ferrous sulfate/ferrous nitrate, ferrous sulfate etc. such as, preferred ferrous nitrate and/or ferrous sulfate, and further preferably sulfuric acid is ferrous.
The salt of silver salt of the present invention to be cation be silver ion, anyly all can be used for the present invention by silver salt soluble in water, such as silver nitrate, silver acetate etc.The preferred silver nitrate of silver salt of the present invention and/or silver acetate, further preferred silver nitrate.
As optimal technical scheme, the preparation method of silver-colored micro-/ nano line of the present invention comprises the steps:
(1) get silver salt, reducing agent and template to be dissolved in the water respectively, prepare silver salt solution, the reducing agent aqueous solution and the template aqueous solution;
(2) template is joined in silver salt solution, heating and thermal insulation;
(3) reducing agent is dripped in the solution obtained to step (2);
(4) dropwise, centrifugation must precipitate, through washing, dry silver-colored micro-/ nano line.
Preparation process of the present invention is by silver salt and citrate complexing, and the product then complexing obtained reduces, and under the effect of citrate as template, prepares silver-colored micro-/ nano line.Reaction temperature required for the present invention is not high, and carry out, in the process of reducing, needing heating and thermal insulation at dropping reducing agent, the temperature of insulation is 40-60 DEG C, such as 40 DEG C, 42 DEG C, 47 DEG C, 53 DEG C, 58 DEG C, 60 DEG C etc., preferred 45-55 DEG C, preferably 50 DEG C further.
The outward appearance of speed on the silver-colored micro-/ nano line prepared dripping reducing agent also has impact, in order to prepare the larger silver-colored micro-/ nano line of draw ratio, the speed of the described dropping reducing agent of rate-determining steps of the present invention (3) is 0.1-0.5mL/min, such as 0.10mL/min, 0.11mL/min, 0.13mL/min, 0.25mL/min, 0.29mL/min, 0.35mL/min, 0.38mL/min, 0.44mL/min, 0.50mL/min etc., preferred 0.2-0.35mL/min, further preferred 0.33mL/min.
If the concentration of silver salt, reducing agent is too high in the present invention, cause effects of ion excessive concentration, the complexing of citrate ion is consumed by other ions except silver ion, causes the waste of citrate ion; If the concentration of silver salt, reducing agent is too low, cause the growth insufficient raw material of silver-colored micro-/ nano line, cause the length of silver-colored micro-/ nano line shorter.
Preferably, in step of the present invention (1), the concentration of silver salt solution is 0.5-5.0g/L, such as 0.5g/L, 0.8g/L, 1.2g/L, 1.8g/L, 2.0g/L, 2.7g/L, 3.2g/L, 3.8g/L, 4.5g/L, 5.0g/L etc., preferred 1.0g/L-3.5g/L.
Preferably, the concentration of the described reducing agent aqueous solution of step of the present invention (1) is 2g/L-10g/L, and such as 2.0g/L, 2.2g/L, 2.9g/L, 3.5g/L, 3.9g/L, 4.3g/L, 4.8g/L, 5.9g/L, 6.4g/L, 7.0g/L, 8.7g/L, 9.8g/L, 10g/L etc. are 2-8g/L preferably.
In the present invention, the excessive or too small waste that all can cause raw material of the ratio of reducing agent and silver salt.Therefore, the mass ratio of the preferred described reducing agent of the present invention and silver salt is (5-1): 1, such as 5: 1,4.8: 1,4.0: 1,3.7: 1,3.2: 1,2.5: 1,2.1: 1,1.7: 1,1.3: 1,1: 1 etc., preferably (3.5-1): 1.
The concentration of step of the present invention (1) described template in silver salt solution is 0.5-5g/L, such as 0.5g/L, 0.6g/L, 0.9g/L, 1.1g/L, 1.6g/L, 2.6g/L, 3.3g/L, 4.1g/L, 4.8g/L, 5.0g/L, preferred 1.0-3.5g/L;
Preferably, in deionized water, distilled water and redistilled water a kind of described wet concentration.
As optimal technical scheme, the wet chemical preparation method of silver-colored micro-/ nano line of the present invention comprises the steps:
(1) silver nitrate ferrous sulfate and citric acid are dissolved in deionized water respectively, obtain silver nitrate aqueous solution, ferrous sulfate aqueous solution and aqueous citric acid solution;
(2) aqueous citric acid solution is joined in silver nitrate aqueous solution, heating gained mixed solution, insulation, control temperature is at 40-60 DEG C;
(3) to the mixed solution and dripping ferrous sulfate that step (2) obtains, rate of addition is 0.1-0.3mL/min;
(4) dropwise, centrifugation must precipitate, through washing, dry silver-colored micro-/ nano line.
As alternatives, the wet chemical preparation method of silver-colored micro-/ nano line of the present invention comprises the steps: respectively appropriate silver nitrate, ferrous sulfate and citric acid to be dissolved into wiring solution-forming in deionized water.Then in liquor argenti nitratis ophthalmicus, drip the citric acid solution of appropriate amount, form the liquor argenti nitratis ophthalmicus containing citric acid.Then this solution is heated to 50 DEG C, keeps constant, and in this solution, drip appropriate copperas solution with suitable rate of addition.After dropwising, from solution, isolate sediment, wash 3-4 time successively with water and absolute alcohol, eventually pass vacuum drying and obtain silver-colored micro wire.
Two of object of the present invention is to provide a kind of silver-colored micro-/ nano line, and described silver-colored micro-/ nano line is prepared by the method for the invention.Diameter≤0.6 micron of the silver-colored micro-/ nano line that the present invention prepares, preferred diameter is 0.2-0.6 micron; Length-controllable is 3-30 micron.
Compared with prior art, the present invention has following beneficial effect:
(1) operating temperature of the method for the invention is low, whole process all can be able to be carried out below 60 DEG C, compared with prior art, reaction temperature reduces greatly, not only save the energy, provide cost savings, and greatly reduce the difficulty of operation, improve the security preparing silver-colored micro-/ nano line.The reacting phase ratio of such as, in the wet chemical methods of reporting for work with Caswell etc. 100 DEG C, reaction temperature reduces greatly.
(2) the present invention does not add any macromolecule dispersant, carries out completely in an aqueous medium, does not produce harmful substance, very environmental protection.
(3) process of preparing of silver-colored micro-/ nano line provided by the invention, simple to operate, easily control, there is very wide industrial prospect.
Accompanying drawing explanation
The silver-colored micro-/ nano line of Fig. 1 prepared by embodiment one amplifies the SEM figure of 2000 times;
The silver-colored micro-/ nano line of Fig. 2 prepared by embodiment one amplifies the SEM figure of 3000 times;
The XRD figure of the silver-colored micro-/ nano line of Fig. 3 prepared by embodiment one;
Fig. 4 is the SEM figure that embodiment two gained silver micro-/ nano line amplifies 2000 times;
Fig. 5 is the SEM figure that embodiment three gained silver micro-/ nano line amplifies 2000 times.
Detailed description of the invention
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
21mg silver nitrate and 50mg ferrous sulfate are dissolved in 10mL deionized water respectively, 19.2mg citric acid are dissolved in 3mL deionized water and are made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 50 DEG C, then toward this mixed solution and dripping 8mL copperas solution, after dropwising in 30min (rate of addition 0.33mL/min), centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro-/ nano line.Fig. 1 is the SEM figure that embodiment one gained silver micro-/ nano line amplifies 2000 times; Fig. 2 is the SEM figure that embodiment one gained silver micro-/ nano line amplifies 3000 times; Fig. 3 is the XRD figure of embodiment one gained silver micro-/ nano line.
Embodiment two
10.5mg silver nitrate and 50mg ferrous sulfate are dissolved in 10mL deionized water respectively, 19.2mg citric acid are dissolved in 3mL deionized water and are made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 50 DEG C, then toward this mixed solution and dripping 5mL copperas solution, after dropwising in 30min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro wire.Fig. 4 is the SEM figure that embodiment two gained silver micro-/ nano line amplifies 2000 times.
Embodiment three
30mg silver nitrate and 100mg ferrous sulfate are dissolved in 10mL deionized water respectively, 32mg citric acid and disodium citrate 10mg are dissolved in 3mL deionized water and are made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 60 DEG C, then toward this mixed solution and dripping 5mL copperas solution, after dropwising in 30min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro wire.Fig. 5 is the SEM figure that embodiment three gained silver micro-/ nano line amplifies 2000 times.
Embodiment four
5mg silver nitrate and 10mg ferrous sulfate are dissolved in 10mL deionized water respectively, 5mg potassium citrate are dissolved in 3mL deionized water and are made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 40 DEG C, then toward this mixed solution and dripping 5mL copperas solution, after dropwising in 50min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro-/ nano line.The diameter of the nano silver wire obtained is 0.6 micron, and length-controllable is 150 microns.
Embodiment five
4mg silver nitrate is dissolved into 8mL deionized water and 30mg ferrous sulfate is dissolved in 3mL deionized water, 4mg potassium citrate is dissolved in 3mL ionized water and is made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 60 DEG C, then toward this mixed solution and dripping 2mL copperas solution, after dropwising in 20min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro-/ nano line.The diameter of the nano silver wire obtained is 0.3 nanometer, and length-controllable is 30 microns.
Embodiment six
20mg silver nitrate is dissolved into 4ml deionized water and 30mg ferrous sulfate is dissolved in 30mL deionized water, 20mg potassium citrate is dissolved in 3mL deionized water and is made into citric acid solution.After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 60 DEG C, then toward this mixed solution and dripping 20mL copperas solution, after dropwising in 40min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro-/ nano line.The diameter of the nano silver wire obtained is 0.2 micron, and length-controllable is 12 microns.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (1)
1. a preparation method for silver-colored micro-/ nano line, is characterized in that, described method, for be dissolved in 10mL deionized water respectively by 5mg silver nitrate and 10mg ferrous sulfate, to be dissolved into 5mg potassium citrate in 3mL deionized water and to be made into citric acid solution; After citric acid solution is added liquor argenti nitratis ophthalmicus, this mixed solution is heated, make it to remain on 40 DEG C, then toward this mixed solution and dripping 5mL copperas solution, after dropwising in 50min, centrifugation precipitates, after spending deionized water several times, with absolute ethanol washing 2-3 time, last vacuum drying obtains silver-colored micro-/ nano line;
The diameter of described silver-colored micro-/ nano line is 0.6 micron, and length-controllable is 150 microns.
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| CN105290420B (en) * | 2012-11-29 | 2017-11-21 | 江苏理工学院 | The method for preparing flaky nanometer silver powder |
| CN103273082B (en) * | 2013-06-13 | 2015-02-18 | 昆山西微美晶电子新材料科技有限公司 | Flower-like spherical silver powder preparing method |
| CN104625084B (en) * | 2014-12-31 | 2016-08-24 | 烟台佳隆纳米产业有限公司 | A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol |
| CN104607655B (en) * | 2015-03-06 | 2016-08-24 | 苏州大学 | A kind of preparation method of nano silver wire |
| CN106694899B (en) * | 2016-11-15 | 2018-07-03 | 西南科技大学 | A kind of preparation method of the controllable silver nanoparticle spool of size |
| CN108655414A (en) * | 2018-06-11 | 2018-10-16 | 合肥学院 | A kind of quick magnanimity prepares the simple and easy method of two dimension Ag micro Nano materials |
| CN109604633A (en) * | 2018-12-28 | 2019-04-12 | 广东银研高新材料股份有限公司 | A kind of preparation method of nano-silver thread |
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