CN108994315B - Method for preparing silver nanowire material by using carrageenan as template and reducing agent - Google Patents
Method for preparing silver nanowire material by using carrageenan as template and reducing agent Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 26
- 235000010418 carrageenan Nutrition 0.000 title claims abstract description 24
- 229920001525 carrageenan Polymers 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 title claims abstract description 21
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 title claims abstract description 21
- 239000000679 carrageenan Substances 0.000 title claims abstract description 20
- 229940113118 carrageenan Drugs 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000011541 reaction mixture Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims 1
- 238000012512 characterization method Methods 0.000 abstract description 2
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 230000007935 neutral effect Effects 0.000 description 7
- 238000000926 separation method Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
A method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent relates to the technical field of electronic material application. According to the mass ratio of 1-3: weighing carrageenin and silver nitrate in a beaker, adding ionized water for mixing and dissolving, then adding diluted acid to adjust the pH value to be below 6, and adding the mixture into an ultrasonic cleaner for ultrasonic treatment; and transferring the reaction mixed solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into a constant-temperature air blast oven for reaction, and performing post-treatment after the reaction to obtain the silver nanowire material. The invention mainly takes carrageenan as a template and a reducing agent, and silver nitrate is reduced into silver nanowires with high length-diameter ratio under hydrothermal condition. According to the invention, carrageenan and silver nitrate are used as reaction raw materials, and the silver nanowire with high length-diameter ratio is prepared in one step by a hydrothermal method. Through serial characterization, the high-aspect ratio silver nanowire material is obtained.
Description
Technical Field
The invention relates to the technical field of electronic material application, in particular to a method for preparing a silver nanowire material by using carrageenan as a template and a reducing agent.
Background
Silver has found wide application in catalysis, electronics, optics, and information storage, etc. due to its unique physicochemical properties. Particularly, silver nanowires are one of key materials for manufacturing conductive ink in the full-printed electronic technology, and have been applied to the fields of materials of transparent electrodes, thin-film solar cells and the like along with the improvement of the electronic technology and the improvement of the integration level of electronic products.
At present, templates mainly comprise polyvinylpyrrolidone (PVP), quaternary ammonium salt cations and hexadecyl trimethyl ammonium bromide in the preparation process of silver nanowires, and reducing agents such as glucose or ethylene glycol are added, so that the preparation process is complicated, and the product after reaction has certain toxicity and causes environmental pollution.
Disclosure of Invention
The invention aims to provide a method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent, which has the advantages of simple process, low cost and suitability for industrial mass production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent comprises the following steps:
1) preparation of reaction mixture
According to the mass ratio of 1-3: weighing carrageenin and silver nitrate in a beaker, adding ionized water for mixing and dissolving, then adding diluted acid to adjust the pH value to be below 6, and adding the mixture into an ultrasonic cleaner for ultrasonic treatment;
2) hydrothermal reaction of
And transferring the reaction mixed solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into a constant-temperature air blast oven for reaction, and performing post-treatment after the reaction to obtain the silver nanowire material.
As a preferred technical scheme of the method for preparing the silver nanowire material by using the carrageenan as the template and the reducing agent, the ultrasonic treatment time in the ultrasonic cleaner in the step 1) is 0.5-2 h, the hydrothermal reaction temperature in the step 2) is 140-180 ℃, and the reaction time is 8-16 h. And in the post-treatment in the step 2), the reaction product is subjected to solid-liquid separation, then is alternately washed by absolute ethyl alcohol and deionized water, and then is placed in a constant-temperature drying oven for drying, wherein the drying temperature in the constant-temperature drying oven is 40-80 ℃, and the drying time is 6-18 hours.
The invention mainly takes carrageenan as a template and a reducing agent, and silver nitrate is reduced into silver nanowires with high length-diameter ratio under hydrothermal condition. According to the invention, carrageenan and silver nitrate are used as reaction raw materials, and the silver nanowire with high length-diameter ratio is prepared in one step by a hydrothermal method. Through serial characterization, the high-aspect ratio silver nanowire material is obtained.
Compared with the prior art, the invention also has the following advantages:
1) the method has the advantages of simple process, easy construction of the whole preparation system, simple and convenient operation, easy control of conditions and low cost, and is suitable for large-scale industrial production.
2) The invention adopts the carrageenan as the template and the reducing agent, produces few byproducts in the preparation process, and is an environment-friendly synthesis process.
Drawings
The method for preparing silver nanowire material using carrageenan as template and reducing agent according to the present invention is further described in detail below with reference to the following examples and accompanying drawings.
FIG. 1 is a photograph showing a comparison of appearance of the mixed solution of lacca gum and silver nitrate at different pH values in example 1, and FIGS. 1a, b, and c correspond to the mixed solution of acid, neutral and alkali in sequence.
FIG. 2 is SEM images of products prepared from mixed solutions of lacca and silver nitrate at different pH values in example 1, and FIGS. 2a, b and c correspond to acidic, neutral and alkaline mixed solutions in sequence.
FIG. 3 is an SEM photograph of a product prepared in example 2.
FIG. 4 is a scanning electron microscopy spectroscopy analysis of the product prepared in example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1
A method for preparing silver nano material by taking carrageenan as a template and a reducing agent comprises the following steps:
1) preparation of reaction mixture
The experiment is divided into three groups, 1g of carrageenin and 0.5g of silver nitrate are weighed in each group, 90mL of ionized water is added for mixing and dissolving, the pH value of the group 1 is adjusted to 6 (acid group) by adding dilute hydrochloric acid, the pH value of the group 2 is not adjusted (neutral group), the pH value of the group 3 is adjusted to 9 (alkaline group) by adding sodium hydroxide solution, and then the groups are respectively added into an ultrasonic cleaner for ultrasonic treatment for 1 h.
FIG. 1 is a photograph showing a comparison of appearance of the mixed solution of lacca gum and silver nitrate at different pH values in example 1, and FIGS. 1a, b, and c correspond to the mixed solution of acid, neutral and alkali in sequence. As can be seen by comparison of fig. 1: under the acidification and neutral conditions, silver nitrate and carrageenan form a compound white colloidal substance, and under the alkaline condition, the black brown silver oxide is separated from the carrageenan template to form a precipitate.
2) Hydrothermal reaction of
Respectively transferring the reaction mixed liquid into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into a constant-temperature air-blast oven for reaction, setting the hydrothermal reaction temperature at 140 ℃ and setting the reaction time at 16 h. After the reaction, the reaction products are respectively washed alternately by absolute ethyl alcohol and deionized water after solid-liquid separation, and then are dried for 6 hours in a constant temperature drying oven at the temperature of 80 ℃.
FIG. 2 is SEM images of products prepared from mixed solutions of lacca and silver nitrate at different pH values in example 1, and FIGS. 2a, b and c correspond to acidic, neutral and alkaline mixed solutions in sequence. As can be seen from fig. 2, the product prepared under acidic condition is a nanowire-like substance, the product prepared under alkaline condition is a nanoparticle-like substance, and the product prepared under neutral condition is a mixed and interlaced form of nanowires and nanoparticles.
Example 2
A method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent comprises the following steps:
1) preparation of reaction mixture
1.2g of carrageenan and 0.5g of silver nitrate are weighed in each group, added with 90mL of ionized water for mixing and dissolving, then added with dilute hydrochloric acid to adjust the pH value to 5, and added into an ultrasonic cleaner for ultrasonic treatment for 2 hours.
2) Hydrothermal reaction of
Transferring the reaction mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and putting the reaction kettle into a constant-temperature air-blast oven for reaction, wherein the hydrothermal reaction temperature is 160 ℃, and the reaction time is 12 hours. After the reaction, the reaction product is subjected to solid-liquid separation, then is alternately washed by absolute ethyl alcohol and deionized water, and then is dried in a constant-temperature drying oven at 60 ℃ for 12 hours to obtain the silver nanowire material.
FIG. 3 is an SEM photograph of a product prepared in example 2, and FIG. 4 is a scanning electron microscopy energy spectrum analysis photograph of the product prepared in example 2. As can be seen from fig. 3 and 4, the silver nano-product with almost uniform diameter less than about 50 nm and length up to several microns is obtained in this example, i.e. the silver nano-wire with high aspect ratio is obtained.
Example 3
A method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent comprises the following steps:
1) preparation of reaction mixture
0.5g of carrageenan and 0.5g of silver nitrate are weighed in each group, mixed and dissolved by adding 90mL of ionized water, then diluted hydrochloric acid is added to adjust the pH value to 4, and the mixture is added into an ultrasonic cleaner for ultrasonic treatment for 0.5 h.
2) Hydrothermal reaction of
Transferring the reaction mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and putting the reaction kettle into a constant-temperature air-blast oven for reaction, wherein the hydrothermal reaction temperature is 180 ℃, and the reaction time is 8 h. After the reaction, the reaction product is subjected to solid-liquid separation, then is alternately washed by absolute ethyl alcohol and deionized water, and then is dried in a constant-temperature drying oven at 40 ℃ for 18 hours to obtain the silver nanowire material.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (3)
1. A method for preparing a silver nanowire material by taking carrageenan as a template and a reducing agent is characterized by comprising the following steps:
1) preparation of reaction mixture
According to the mass ratio of 1-3: weighing carrageenin and silver nitrate in a beaker, adding ionized water for mixing and dissolving, then adding diluted acid to adjust the pH value to be below 6, and adding the mixture into an ultrasonic cleaner for ultrasonic treatment for 0.5-2 h;
2) hydrothermal reaction of
Transferring the reaction mixed solution into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into a constant-temperature air-blast oven for reaction, wherein the hydrothermal reaction temperature is 140-180 ℃, the reaction time is 8-16 h, and carrying out post-treatment after the reaction to obtain a silver nanowire material;
the diameter of the prepared silver nanowire material is less than 50 nm.
2. The method as claimed in claim 1, wherein the post-treatment in step 2) is to separate the solid from the liquid of the reaction product, wash the reaction product alternately with absolute ethyl alcohol and deionized water, and then dry the reaction product in a constant-temperature drying oven.
3. The method of claim 2, wherein the drying temperature in the constant-temperature drying oven is 40-80 ℃ and the drying time is 6-18 h.
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| CN109759603B (en) * | 2019-03-19 | 2022-01-18 | 合肥学院 | Method for preparing silver nanowires by utilizing actinomycetes |
| CN111375760B (en) * | 2020-04-28 | 2022-06-28 | 中国科学院海洋研究所 | Au-Ag nano core-shell material using carrageenan as reducing agent and preparation method and application thereof |
| CN114505489A (en) * | 2020-10-27 | 2022-05-17 | 深圳市华科创智技术有限公司 | Preparation method of silver nanowires |
Citations (4)
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|---|---|---|---|---|
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
| JP2008081750A (en) * | 2005-09-08 | 2008-04-10 | Univ Kinki | Composite body obtained by including metal particulate with polysaccharide, and its applied product |
| CN104625087A (en) * | 2015-02-28 | 2015-05-20 | 济宁利特纳米技术有限责任公司 | Method for hydrothermally manufacturing silver nanowires |
| CN106041115A (en) * | 2016-05-26 | 2016-10-26 | 华南理工大学 | Sodium alga acid/silver nanowire sol and preparation method thereof |
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| US20130090237A1 (en) * | 2011-10-11 | 2013-04-11 | Sanat Mohanty | Pteredin pentanedioic derivative based nanoparticles |
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|---|---|---|---|---|
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
| JP2008081750A (en) * | 2005-09-08 | 2008-04-10 | Univ Kinki | Composite body obtained by including metal particulate with polysaccharide, and its applied product |
| CN104625087A (en) * | 2015-02-28 | 2015-05-20 | 济宁利特纳米技术有限责任公司 | Method for hydrothermally manufacturing silver nanowires |
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| Title |
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