CN105386119A - Preparation method of dendritic silver nanocrystalline coating using electrodeposition - Google Patents
Preparation method of dendritic silver nanocrystalline coating using electrodeposition Download PDFInfo
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- CN105386119A CN105386119A CN201510717860.1A CN201510717860A CN105386119A CN 105386119 A CN105386119 A CN 105386119A CN 201510717860 A CN201510717860 A CN 201510717860A CN 105386119 A CN105386119 A CN 105386119A
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- electrode
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- galvanic deposit
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/12—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by electrolysis
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/66—Crystals of complex geometrical shape, e.g. tubes, cylinders
Abstract
The present invention discloses a preparation method of a dendritic silver nanocrystalline coating using electrodeposition. Metal wire is successively subjected to acetone and ultrapure water ultrasonic washing and the washed metal wire is immersed into a strong acid solution to conduct etching. Then silver salt solution is used as an electrolyte, the processed metal wire is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum electrode as a counter electrode, and voltage, scanning number and scanning rate are controlled to conduct electrodeposition. The product is taken out and washed by the ultrapure water and the washed product is dried with air isolation to obtain the homogeneous dendritic silver nanocrystalline. The sizes of the silver nanocrystallines are between 1[mu]m-6[mu]m and the silver nanocrystallines are stable in quality. The method is used to extract polycyclic aromatic hydrocarbons (PAHs) in the environmental samples with a high extraction efficiency. Besides, the size and morphology of the silver nanocrystalline can be controlled by selecting the voltage, the scanning number and the scanning rate, and the preparation process is simple, the cost is low and the operability is strong.
Description
Technical field
Method, be mainly used in the coating of extracting head in solid phase micro-extraction technique, belong to field of nanometer material technology and environmental analysis Material Field.
Background technology
Solid phase micro-extraction technique (SolidPhaseMicroextraction, SPME) is a kind of novel without the need to solvent, simple to operate, time saving and energy saving analytical technology, extensively obtains the favor of analyst.Extracting head is the core of SPME, and the performance of the coating of extracting head and extracting head has close relationship, and the character of coating determines the sensitivity of analytical procedure, the selectivity of extraction and the repeatability of mensuration.But the shortcomings such as price is high, kind is few, the life-span is short, poor stability that current solid-phase micro-extraction coating also exists.Therefore, the coated material developing high efficiency low cost has very important significance and using value.Wherein noble metal nanometer material is especially because it has stable performance and special physicochemical property have good development prospect.
Along with people are to the research of noble metal nanometer material, the noble metal nanometer material of a lot of shape and size has been had to synthesize successfully and be widely used.For nano metal material, because its particle is in dispersion state, so improve its surface-area to a certain extent, for the catalyzed reaction in chemical reaction, there is important Research Significance.Compare with general nano material, the nano metal material of branched structure all has highdensity angle, limit and ladder atom, so have higher specific activity and specific surface area, also extend the Utilization prospects of dendritic noble metal nanometer material simultaneously, in catalyzer, SERS and photoluminescence etc., have potential application.
Silver nanoparticle crystalline substance has unique performance, and have widespread use in fields such as catalyzer, electro-conductive material, sensor and antiseptic-germicides, its synthesis method mainly contains chemical reduction method, supersonic method, electrochemical reducing and photoreduction met hod etc.These methods have its respective merits and demerits, and not all method is all suitable for preparing all types of nano material.And electrodip process is the alternative method of the many nanocrystalline materials of preparation, the nanocrystalline material formation time prepared with electrodip process is short, stable in properties, and therefore electrodip process has prepared one of the most promising method of fully dense nano material.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing galvanic deposit to prepare dendroid silver nanoparticle crystal coating, to reduce the preparation cost of silver nanoparticle crystal coating, and improve the stability of silver nanoparticle crystal coating and the life-span short.
The method of dendroid silver nanoparticle crystal coating is prepared in galvanic deposit of the present invention, comprises following processing step:
(1) first use acetone ultrasonic cleaning wire 8min ~ 20min, then use ultrapure water ultrasonic cleaning 5min ~ 10min; Then, at 30 DEG C ~ 50 DEG C, wire is immersed in the strong acid solution of mass concentration 20% ~ 40% and etch 40min ~ 60min.Described wire is the Stainless Steel Wire of Φ=0.25mm ~ 0.45mm, aluminium wire, copper wire or titanium silk.Strong acid is sulfuric acid, hydrochloric acid or hydrofluoric acid;
(2) with 1mmol/L ~ 4mmol/L silver salt solution for electrolytic solution, with the wire of above-mentioned process for working electrode, saturated calomel electrode is reference electrode, and platinum electrode is to electrode, under three-electrode system, carry out galvanic deposit, obtains dendroid silver nanoparticle brilliant.Described silver salt is Sulfuric acid disilver salt or Silver Nitrate.The voltage of described galvanic deposit is-1.2V ~ 1.0V, and the scanning number of turns is that 5 circle ~ 80 are enclosed, and scanning speed is 5mv/s ~ 100mv/s;
(3) brilliant for preparation dendroid silver nanoparticle taking-up ultrapure water is cleaned, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.
Scanning electron microscope analysis shows, silver nanoparticle prepared by the present invention crystalline substance in even dendroid, the size of silver nanoparticle crystalline substance between 1 μm ~ 6 μm, steady quality; For extracting polycyclic aromatic hydrocarbons in environmental sample (PAHs), extraction efficiency is high.And the size of silver nanoparticle crystalline substance and pattern control by selecting voltage, the scanning number of turns and scanning speed.In addition, electrochemical deposition process wire, as carrier, shows good mechanical stability and repeatability compared with traditional fused silica fiber.
Accompanying drawing explanation
Fig. 1 is that example 1 galvanic deposit products therefrom SEM of the present invention schemes.
Fig. 2 is that example 2 galvanic deposit products therefrom SEM of the present invention schemes.
Fig. 3 is that example 3 galvanic deposit products therefrom SEM of the present invention schemes.
Fig. 4 is that example 4 galvanic deposit products therefrom SEM of the present invention schemes.
Fig. 5 is that example 4 galvanic deposit products therefrom EDS of the present invention schemes.
Embodiment
Below by specific embodiment, the method that the present invention prepares dendroid silver nanoparticle crystal coating is described further.
Embodiment 1
(1) first use acetone ultrasonic cleaning titanium silk (Φ=0.25mm) 15min, then use ultrapure water ultrasonic cleaning 8min; Then at 40 DEG C, titanium silk is immersed in the wang aqueous solution of mass concentration 30% and etch 50min, take out, be placed in methanol solution and preserve;
(2) with 4mmol/LAg
2sO
4solution is electrolytic solution, with one end titanium silk of above-mentioned process for working electrode, under three-electrode system, (saturated calomel electrode is reference electrode, platinum electrode is to electrode), voltage is between-0.5V ~ 0.2V, the scanning number of turns is 30 circles, and scanning speed is carry out galvanic deposit under 15mv/s, obtains dendroid silver nanoparticle brilliant;
(3) dendroid silver nanoparticle crystalline substance will be prepared and take out ultrapure water cleaning, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.The SEM figure of product is shown in that (left figure to be magnification the be SEM figure of 5,000 times, right figure magnification is the SEM figure under 20,000 times to Fig. 1.）。Can show that the silver nanoparticle crystalline substance of preparation has good configuration of surface by Fig. 1, in dendritic structure, coating is evenly distributed, and specific surface area is large.
Embodiment 2
(1) first use acetone ultrasonic cleaning copper wire (Φ=0.25mm) 10min, then use ultrapure water ultrasonic cleaning 8min; Then, at 45 DEG C, one end of copper wire is immersed in the wang aqueous solution of mass concentration 30% and etch 40min; Take out, be placed in methanol solution and preserve;
(2) with the Ag of 2mmol/L
2sO
4solution is as electrolytic solution, with one end copper wire of above-mentioned process for working electrode, under three-electrode system, (saturated calomel electrode is reference electrode, platinum electrode is to electrode), selection voltage is between-0.2V ~ 0.8V, the scanning number of turns is 20 circles, and scanning speed is carry out galvanic deposit under 50mv/s, obtains dendroid silver nanoparticle brilliant;
(3) the nanotrees dendritic silver fiber head taking-up ultrapure water obtained is cleaned, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.The SEM figure of product is shown in that (left figure to be magnification the be SEM figure of 5,000 times, right figure magnification is the SEM figure under 20,000 times to Fig. 2.）。Can show that the silver nanoparticle crystalline substance of preparation has good configuration of surface by Fig. 2, in dendritic structure, coating is evenly distributed, and specific surface area is large.
Embodiment 3
(1) first use acetone ultrasonic cleaning Stainless Steel Wire (Φ=0.35mm) 15min, then use ultrapure water ultrasonic cleaning 5min; And then etch 30min by the hydrofluoric acid solution of Stainless Steel Wire one end immersion mass concentration 30% at 45 DEG C; Take out, be placed in methanol solution and preserve;
(2) with the AgNO of 3mmol/L
3for electrolytic solution, with the Stainless Steel Wire of one end of above-mentioned process for working electrode, under three-electrode system, (saturated calomel electrode is reference electrode, platinum electrode is to electrode), voltage is chosen as between-0.5V ~ 0.3V, the scanning number of turns is 30 circles, and scanning speed is 30mv/s, and it is brilliant that galvanic deposit obtains dendroid silver nanoparticle;
(3) dendroid silver nanoparticle crystal fiber head will be prepared take out, with cleaning, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.The SEM figure of product is shown in that (left figure to be magnification the be SEM figure of 5,000 times, right figure magnification is the SEM figure under 20,000 times to Fig. 3.）。Can draw by Fig. 3 the configuration of surface that the silver nanoparticle crystalline substance of preparation has had, in dendritic structure, coating is evenly distributed, and specific surface area is large.
Embodiment 4
(1) first use acetone ultrasonic cleaning titanium silk (Φ=0.35mm) 10min, then use ultrapure water ultrasonic cleaning 10min; Then, at 40 DEG C, one end of titanium silk is immersed in the hydrofluoric acid solution of mass concentration 40% and etch 60min; Take out, be placed in methanol solution and preserve;
(2) with the AgNO of 1mmol/L
3solution is electrolytic solution, with the titanium silk of one end of above-mentioned process for working electrode, under three-electrode system, (saturated calomel electrode is reference electrode, platinum electrode is to electrode), voltage is chosen as between-0.3V ~ 0.3V, the scanning number of turns is 20 circles, and scanning speed is 20mv/s, and it is brilliant that galvanic deposit obtains dendroid silver nanoparticle;
(3) the dendroid silver nanoparticle crystal fiber head of preparation is taken out, with ultrapure water cleaning, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.The SEM figure of product is shown in that (left figure to be magnification the be SEM figure of 5,000 times, right figure magnification is the SEM figure under 20,000 times to Fig. 4.）。Can draw by Fig. 4 the configuration of surface that the silver nanoparticle crystalline substance of preparation has had, in dendritic structure, coating is evenly distributed, and specific surface area is large.Fig. 5 is that galvanic deposit products therefrom EDS schemes.Can show that institute's plating coating is silver by Fig. 5.
Claims (5)
1. utilize galvanic deposit to prepare the method for dendroid silver nanoparticle crystal coating, comprise following processing step:
(1) first use acetone ultrasonic cleaning wire 8min ~ 20min, then use ultrapure water ultrasonic cleaning 5min ~ 10min; Then, at 30 DEG C ~ 50 DEG C, wire is immersed in the strong acid solution of mass concentration 20% ~ 40% and etch 40min ~ 60min;
(2) with 1mmol/L ~ 4mmol/L silver salt solution for electrolytic solution, with the wire of above-mentioned process for working electrode, saturated calomel electrode is reference electrode, and platinum electrode is to electrode, under three-electrode system, carry out galvanic deposit, obtains dendroid silver nanoparticle brilliant;
(3) brilliant for preparation dendroid silver nanoparticle taking-up ultrapure water is cleaned, dry under isolated air, obtain uniform dendroid silver nanoparticle brilliant.
2. utilize galvanic deposit to prepare the method for dendroid silver nanoparticle crystal coating as claimed in claim 1, it is characterized in that: described wire is the Stainless Steel Wire of Φ=0.25mm ~ 0.45mm, aluminium wire, copper wire or titanium silk.
3. utilize galvanic deposit to prepare the method for dendroid silver nanoparticle crystal coating as claimed in claim 1, it is characterized in that: described strong acid is sulfuric acid, hydrochloric acid or hydrofluoric acid.
4. utilize galvanic deposit to prepare the method for dendroid silver nanoparticle crystal coating as claimed in claim 1, it is characterized in that: described silver salt is Sulfuric acid disilver salt or Silver Nitrate.
5. utilize galvanic deposit to prepare the method for dendroid silver nanoparticle crystal coating as claimed in claim 1, it is characterized in that: the voltage of described galvanic deposit is-1.2V ~ 1.0V, the scanning number of turns is that 5 circle ~ 80 are enclosed, and scanning speed is 5mv/s ~ 100mv/s.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831778A (en) * | 2016-03-31 | 2016-08-10 | 青岛海尔智能技术研发有限公司 | Washing device and operation method |
| CN105951183A (en) * | 2016-06-18 | 2016-09-21 | 合肥松雷信息科技有限公司 | Preparation method of silver nanometer dendrites |
| CN106757173A (en) * | 2016-11-25 | 2017-05-31 | 电子科技大学 | A kind of preparation method of the micro-nano crystal of silver-colored polyhedron without surface ligand |
| CN107084970A (en) * | 2017-05-03 | 2017-08-22 | 中北大学 | A kind of three-dimensional circulated gases SERS detections substrate and preparation method and application |
| CN107389775A (en) * | 2017-08-30 | 2017-11-24 | 大连大学 | A kind of flexible L phenylalanines electrochemical sensor based on dendritic nano-silver structure |
| CN108364806A (en) * | 2018-02-09 | 2018-08-03 | 中山大学 | A kind of tree-shaped three-dimensional structure metal material and preparation method thereof and application in the battery |
| CN108652618A (en) * | 2017-03-30 | 2018-10-16 | 深圳先进技术研究院 | A kind of microelectrode array and preparation method thereof of dendrite platinum modification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831778A (en) * | 2016-03-31 | 2016-08-10 | 青岛海尔智能技术研发有限公司 | Washing device and operation method |
| CN105951183A (en) * | 2016-06-18 | 2016-09-21 | 合肥松雷信息科技有限公司 | Preparation method of silver nanometer dendrites |
| CN106757173A (en) * | 2016-11-25 | 2017-05-31 | 电子科技大学 | A kind of preparation method of the micro-nano crystal of silver-colored polyhedron without surface ligand |
| CN108652618A (en) * | 2017-03-30 | 2018-10-16 | 深圳先进技术研究院 | A kind of microelectrode array and preparation method thereof of dendrite platinum modification |
| CN108652618B (en) * | 2017-03-30 | 2021-09-07 | 深圳先进技术研究院 | Dendritic platinum modified microelectrode array and preparation method thereof |
| CN107084970A (en) * | 2017-05-03 | 2017-08-22 | 中北大学 | A kind of three-dimensional circulated gases SERS detections substrate and preparation method and application |
| CN107389775A (en) * | 2017-08-30 | 2017-11-24 | 大连大学 | A kind of flexible L phenylalanines electrochemical sensor based on dendritic nano-silver structure |
| CN107389775B (en) * | 2017-08-30 | 2020-06-02 | 大连大学 | Flexible L-phenylalanine electrochemical sensor based on dendritic nano-silver structure |
| CN108364806A (en) * | 2018-02-09 | 2018-08-03 | 中山大学 | A kind of tree-shaped three-dimensional structure metal material and preparation method thereof and application in the battery |
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Application publication date: 20160309 |