CN105057695A - Method for preparing silver nanowire by utilizing ionothermal method - Google Patents
Method for preparing silver nanowire by utilizing ionothermal method Download PDFInfo
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- CN105057695A CN105057695A CN201510602083.6A CN201510602083A CN105057695A CN 105057695 A CN105057695 A CN 105057695A CN 201510602083 A CN201510602083 A CN 201510602083A CN 105057695 A CN105057695 A CN 105057695A
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Abstract
The invention discloses a method for preparing a silver nanowire by utilizing an ionothermal method. The method comprises the following steps: firstly weighing proper amount of choline chloride, urea and silver nitrate respectively, putting the materials in an agate grinding bowl to be ground until the two kinds of salt is mixed uniformly and the mixture becomes transparent gel, then transferring the mixture to a polytetrafluoroethylene lining, adding slightly excessive hydrazine hydrate as a reducing agent, then putting the polytetrafluoroethylene lining in an autoclave again, taking out the reaction kettle after reacting at 120-180 DEG C for 2-10 hours, taking out the product after the reaction kettle is naturally cooled to the room temperature, washing the product multiple times and carrying out vacuum drying on the product, thus finally obtaining the silver nanowire with a one-dimensional structure. The method has the technical effects that the method is simple to operate and easy to control, has good repeatability and is environment-friendly, and any surfactant or solvent is not used.
Description
Technical field
The invention belongs to the field of the hot legal system of ion for nano particle of low temperature eutectic solvent, be specifically related to a kind of hot legal system of the ion of low temperature eutectic solvent that utilizes for the method for nano-silver thread.
Background technology
Argent is face-centred cubic structure, and have good soft paving property and ductility, ductility is only second to gold, can be pressed into thin slice, pull into filament.And its electric conductivity and conductivity of heat are all the highest in all metals.Silver also for alloyage, pure medicine, silver foil, silver salt, chemical apparatuses etc., and for silver coin processed and the end silver etc. aspect.
Be different from block silver, Nano Silver is paid close attention to widely because having a lot of unique process based prediction model.At optical field, the plasma resonance on Nano Silver surface or band-to-band transition feature make Nano Silver can send the light of different colours; At electronic applications, excellent conduction and heat conductivility can as transmission medium and conducting mediums by Nano Silver; In medical, Nano Silver can be used as anti-biotic material, molecular diagnosis and gene and treats; In catalysis, the Nano Silver that particle diameter is little, surface area is large is very easily combined with other atom thus shows fabulous catalytic activity and reaction selectivity.Have bibliographical information, why Nano Silver possesses the performance of these excellences, depends primarily on a series of physical parameter, as size, pattern and structure etc.Therefore how better to control Nano Silver performance and obtain the attention that single controlled, the uniform Nano Silver of pattern is day by day subject to researcher.Red shift can be there is in long axis direction plasma resonance (SPR) pattern of such as Nano Silver rod along with the increase of the draw ratio of Nano Silver rod.In recent years, some scholar nanotube of big L/D ratio that utilized the preparation methods such as hydro-thermal method to synthesize; Some scholar uses fluorescence to irradiate BSPP solution and obtains Nano Silver triangular prism; Under some scholar's disodium EDTA (EDTA) existent condition, diamine reduction-oxidation silver is utilized to generate Nano Silver hexagonal sheet.In addition, more scholar is also had also to further investigate the nano-silver thread how preparing big L/D ratio.
The same with other nano metal, the preparation method preparing Nano Silver also has a lot, is generally divided into Physical, chemical method also has bioanalysis.Well-known Physical comprises mechanical attrition method, atomization condensation is sent out, atomization etc., bioanalysis is the emerging preparation method adopting biomaterial or living things system natural synthesis of nano particulate, and chemical method comprises chemical reduction method, microemulsion method, sol-gel processing and the hot method of plasma etc.The hot method of its intermediate ion refers to that the hot method of ion is a kind of novel synthesis methods for nanoparticles that is medium with ionic liquid or eutectic mixture, it provides a kind of unique synthetic environment of ionic state.The advantages such as it has that vapour pressure is little, not volatile, the polarity of Heat stability is good, reusable edible, ionic liquid and hydrophobic/hydrophily can obtain simply by regulating the combination of suitable anion/cation.
Summary of the invention
The object of the present invention is to provide a kind of hot legal system of ion that utilizes for the method for the nano-silver thread of one-dimentional structure, involved equipment and process is simple, does not need to control in course of reaction.
The present invention solves the problems of the technologies described above adopted technical scheme, and a kind of hot legal system of ion that utilizes, for the method for nano-silver thread, is characterized in that comprising the steps:
(1) a certain amount of Choline Chloride, urea and silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate little over amount;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will put into the resistance furnace setting temperature in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Preferably, the molar ratio of described Choline Chloride and urea is 1:1 ~ 1:5.
Preferably, the molar ratio of described silver nitrate and hydrazine hydrate is 4:3 ~ 1:2.
Preferably, described design temperature is 120 ~ 180 DEG C, and temperature retention time is 1 ~ 5h.
Described technique effect of the present invention is: the present invention adopts the hot method of ion to prepare nano silver wire, diametrically belong to Nano grade, namely at a below 100nm, have that use equipment is simple, process easily controls and the feature of preparation method's environmental protection, do not need the solvent adding some surfactants or complex component just can control the pattern of Nano Silver, obtain the nano silver wire of nano-scale.
Accompanying drawing explanation
Fig. 1 is the XRD image graph of nano silver wire of the present invention.
The thing phase of product only containing Nano Silver as seen from the figure, without other thing phases.
Fig. 2 is the SEM image graph of nano silver wire of the present invention.
Have the known Nano Silver of figure to be the nano wire of one dimension size, diametrically reaching nano-scale, length is micron level.
Fig. 3 is the EDS image graph of nano silver wire of the present invention.
Product as seen from the figure, except contain the peak of more weak C and O because of oxidation except, the thing phase only containing Nano Silver.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment one
(1) 1mol Choline Chloride, 1mol urea and 0.75mol silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate of 1mol;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will be put into and be set as 120 DEG C of resistance furnaces in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Embodiment two
(1) 1mol Choline Chloride, 2mol urea and 1mol silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate of 1mol;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will be put into and be set as 140 DEG C of resistance furnaces in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Embodiment three
(1) 1mol Choline Chloride, 3mol urea and 1mol silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate of 1.5mol;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will be put into and be set as 160 DEG C of resistance furnaces in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Embodiment four
(1) 1mol Choline Chloride, 4mol urea and 1mol silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate of 1mol;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will be put into and be set as 180 DEG C of resistance furnaces in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Embodiment five
(1) 1mol Choline Chloride, 5mol urea and 1mol silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate of 2mol;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will be put into and be set as 120 DEG C of resistance furnaces in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
Claims (4)
1. utilize the hot legal system of ion for a method for the nano-silver thread of one-dimentional structure, it is characterized in that comprising the steps:
(1) a certain amount of Choline Chloride, urea and silver nitrate are mixed, be fully ground to even transparent glue;
(2) above-mentioned eutectic solvent is put into the liner of the tetrafluoroethene cleaned up, add the hydrazine hydrate little over amount;
(3) polytetrafluoroethyllining lining put into stainless steel cauldron and tighten, reactor will put into the resistance furnace setting temperature in advance;
(4) after above-mentioned reaction to certain hour, cool to room temperature with the furnace, take out reactor, product alcohol and the abundant washing and filtering of deionized water;
(5) by dry for the product vacuum obtained, silvery white Argent grain is obtained.
2. a kind of hot legal system of ion that utilizes according to claim 1 is for the method for nano silver wire, it is characterized in that: the molar ratio of described Choline Chloride and urea is 1:1 ~ 1:5.
3. a kind of hot legal system of ion that utilizes according to claim 1 is for the method for nano silver wire, it is characterized in that: the molar ratio of described silver nitrate and hydrazine hydrate is 4:3 ~ 1:2.
4. a kind of hot legal system of ion that utilizes according to claim 1 is for the method for nano silver wire, and it is characterized in that: described design temperature is 120 ~ 180 DEG C, temperature retention time is 1 ~ 5h.
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Cited By (1)
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CN113714509A (en) * | 2021-09-01 | 2021-11-30 | 西北大学 | Urea-reduced silver nanowire and preparation method and application thereof |
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GB2463878A (en) * | 2008-09-25 | 2010-03-31 | Dca Consultants Ltd | Ionic catalyst capture of carbon oxides |
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WO2015135463A1 (en) * | 2014-03-11 | 2015-09-17 | The Hong Kong University Of Science And Technology | Electrical and thermal conductive paste composition and method of reducing percolation threshold and enhancing percolating conductivity using the same |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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GB2463878A (en) * | 2008-09-25 | 2010-03-31 | Dca Consultants Ltd | Ionic catalyst capture of carbon oxides |
CN102491304A (en) * | 2011-12-02 | 2012-06-13 | 罗绍华 | Method for preparing lithium iron phosphate in ionic eutectic mixture |
WO2015135463A1 (en) * | 2014-03-11 | 2015-09-17 | The Hong Kong University Of Science And Technology | Electrical and thermal conductive paste composition and method of reducing percolation threshold and enhancing percolating conductivity using the same |
CN104399999A (en) * | 2014-12-19 | 2015-03-11 | 南昌航空大学 | Method for preparing hexagonal nanocopper particles by utilizing ionothermal synthesis |
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CN113714509A (en) * | 2021-09-01 | 2021-11-30 | 西北大学 | Urea-reduced silver nanowire and preparation method and application thereof |
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