CN108723388A - A kind of preparation method of silver nanoparticle dendrite - Google Patents

A kind of preparation method of silver nanoparticle dendrite Download PDF

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Publication number
CN108723388A
CN108723388A CN201810684162.XA CN201810684162A CN108723388A CN 108723388 A CN108723388 A CN 108723388A CN 201810684162 A CN201810684162 A CN 201810684162A CN 108723388 A CN108723388 A CN 108723388A
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Prior art keywords
copper rod
silver nanoparticle
distilled water
silver
preparation
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CN201810684162.XA
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Chinese (zh)
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汤瑨
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Hefei Tang Da Mdt Infotech Ltd
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Hefei Tang Da Mdt Infotech Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A kind of preparation method of silver nanoparticle dendrite, which is characterized in that include the following steps:A, copper rod is taken, is cleaned;The cleaning includes the following steps:Under Ultrasonic Conditions, acetone, ethyl alcohol, dilute hydrochloric acid, distilled water cleaning copper rod are used successively;B, silver nanoparticle dendrite is prepared, is included the following steps:(1)Under room temperature, stirring condition, monovalence silver salt is taken to be dissolved in distilled water, obtains solution A;(2)Copper rod obtained by step a is taken, solution A is added dropwise to copper rod, is reacted under normal temperature condition 20-80 seconds, uses distilled water flushing copper rod later, that is, obtain the silver nanoparticle dendrite.The present invention proposes a kind of method of synthesis Ag nanodendrites easy to operate, low-cost.

Description

A kind of preparation method of silver nanoparticle dendrite
Technical field
The invention belongs to heterojunction structure preparation method is grown on copper-based bottom.
Background technology
Diabetes are a kind of since blood glucose builds up then exceeded disease, the title with " killer of silence ", especially It is Adult Onset's patients with type Ⅰ DM.Due to complication, patient's service life can be reduced by suffering from diabetes, in Japan, quadragenarian male by Contributive rate is very high(Account for 10%), it would therefore be desirable to as the early as possible glucose excessive in blood and in time of detecting Control its concentration.
Charge transmission or the variation of the electrical characteristics caused by electrochemical reaction of chemical stages, root are surveyed in electrochemical sensing detection According to induction mechanism, these electrochemical sensors require special electrode, and when test, electrode, which contacts with solution and results from target, to be divided The concentration dependent signal for analysing object, the signal detected needs to amplify or signal processing, the circuit for completing these functions are very convenient Integrated with sensor electrode.
Electrochemical sensor also has religion highly sensitive, and minimum analysis detection limit is up to 10-12Mol/L, instrument and equipment are simpler Single, cheap, the debugging and operation of instrument are all relatively simple, and automation easy to implement needs the amount of reagent few, can be used for micro Operation, the range of measurement is wide, and has good selectivity, reliability and longer life expectancy.It is passed just because of electrochemistry Sensor has the characteristics that these are excellent so that it is applied in many fields, wherein using most in solid state chemistry sensor field Extensively, many solid-state electrochemical sensors have been commercialized, such as glucose sensor, come out it in glucose sensor Before, patient need to instruct insulin injection amount using so-called " the Ban Shi experiment glucoses in urine estimation technique ", this method is quite cumbersome, and The blood glucose of human body is measured with regard to very convenient with electrochemical glucose sensor.
Silver is a kind of important precious metal material, and so far, Ag nanocrystal patterns obtained have much, for example, Nanocube, nano-plates, nano wire, nanometer rods, nano particle etc., in various special nanostructures, Ag nanodendrites It receives extensive attention, because it has larger specific surface area, good connection can be provided, and make these connections can be It works in a variety of applications, such as biosensor, chemical sensor, surface plasma and super-hydrophobic film, with self assembly Layering and the dendritic material etc. for repeating superstructure.It is reported that there are many by electrochemistry, chemically and physically method obtains at present The method of Ag nanodendrites has been disclosed for many silver nanoparticle dendrite processes so far.Chinese patent CN 102181891 A disclose a kind of preparation method with constant current legal system silver nanoparticle dendrite, 102031539 B of Chinese patent CN Disclose a kind of with the preparation method of electrochemical reducting reaction silver nanoparticle dendrite, but method is all comparatively laborious, preparation process It is complex.However, existing most of synthetic methods need reducing agent, high temperature or surfactant, some reducing agents such as boron Sodium hydride is toxic, this can not only damage experimenter, and harm can be also brought to environment, so, it would be desirable to it looks for To a kind of method easy to operate, control is accurate, at low cost, environmentally friendly.The present invention proposes a kind of easy to operate, at low cost The method of honest and clean synthesis Ag nanodendrites.
Invention content
Based on the defect synthesized above, the present invention provides one kind using copper rod as substrate, by regulate and control silver nitrate concentration and Reaction time directly makes silver nanoparticle dendritic growth on copper rod at normal temperatures, can be used as the electrode material for detecting glucose.
Here, a kind of preparation method of silver nanoparticle dendrite provided by the invention, includes the following steps:
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
The above-mentioned copper rod handled well is put into 5mL test tubes at room temperature, instills monovalence silver salt, is reacted 20-80 seconds at normal temperatures, There are the copper rod of atrament, drying at room temperature with distilled water flushing growth, you can, a concentration of 0.03- of the monovalence silver salt 0.06M。
The monovalence silver salt is the AgNO of 0.05M3Solution.
The present invention carries out at normal temperatures, and energy consumption is low, environmentally safe, meets 12 big principles of Green Chemistry.
The copper rod used in the present invention due to its good electric conductivity, cheap price, and can be widely used in copper For the preparation of the heterojunction structure electrode of the various different nano materials of substrate.
The detection that electrochemical sensing property is carried out to electrode prepared by the present invention, is examined in the sodium hydroxide solution of pH=13 Glucose is surveyed, the result shows that the electrode has glucose good electrochemical catalysis effect really, and can be directly used as Fuel cell.
Compared with prior art, the present invention high with reproducibility, material high detection performance is easy to operate, and energy consumption is low, synthesis It is at low cost, it is suitable for industrial extensive preparation;Prepared silver nanoparticle dendrite possesses larger specific surface area, as sensing Equipment material can come into full contact with determinand, keep electrocatalytic reaction fully efficient.
Specific implementation method
Below to the preparation process of the present invention, method and electrochemical applications are described further:
Embodiment 1
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 0.85g silver nitrates are dissolved in the silver nitrate solution that 0.05M is made into the distilled water of 100ml, cross-sectional area For 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.05M silver nitrate solutions of 1ml is taken to instill In test tube, 50s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Embodiment 2
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 0.17g silver nitrates are dissolved in the silver nitrate solution that 0.01M is made into the distilled water of 100ml, cross-sectional area For 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.01M silver nitrate solutions of 1ml is taken to instill In test tube, 50s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Made silver nanoparticle dendrite is considerably less, and also many nano particles generate.
Embodiment 3
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 0.17g silver nitrates are dissolved in the silver nitrate solution that 0.01M is made into the distilled water of 100ml, cross-sectional area For 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.01M silver nitrate solutions of 1ml is taken to instill In test tube, 120s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Made silver nanoparticle dendrite is extremely thick and is packed together.
Embodiment 4
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 0.85g silver nitrates are dissolved in the silver nitrate solution that 0.05M is made into the distilled water of 100ml, cross-sectional area For 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.05M silver nitrate solutions of 1ml is taken to instill In test tube, 5s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Made product does not have dendritic crystalline, entirely particle
Embodiment 5
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 0.85g silver nitrates are dissolved in the silver nitrate solution that 0.05M is made into the distilled water of 100ml, cross-sectional area For 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.05M silver nitrate solutions of 1ml is taken to instill In test tube, 120s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Made silver nanoparticle dendrite shape is similar to example 3.
Embodiment 6
A, the cleaning treatment process of copper rod:
Under ultrasonic cleaning copper rod is cleaned with acetone, ethyl alcohol, 2M hydrochloric acid, distilled water successively;
B, silver nanoparticle dendrite preparation section:
At normal temperatures, 1.7g silver nitrates are dissolved in the silver nitrate solution that 0.1M is made into the distilled water of 100ml, cross-sectional area is 2.5 mm2, length is the cleaned copper rods of 4 cm, and is put into small test tube, and the 0.1M silver nitrate solutions of 1ml is taken to instill test tube In, 50s is reacted at normal temperatures, and distilled water flushing grows the copper rod for having atrament, naturally dry, you can.
Made silver nanoparticle dendrite shape is similar to example 3.
The present invention proposes that a simple method synthesizes silver nanoparticle dendrite on Cu sticks, and obtaining Ag nano materials can be with Directly as electrode.The electrode can not need additional processing under hydrodynamic condition can be effectively performed regeneration, this Show that its reproducibility is good, there is preferable electroxidation ability to also turn out glucose and shows the excellent performance of electrode, so Silver nanoparticle dendrite has the application potential in some novel electrochemical sensors and some other electronic equipment.

Claims (4)

1. a kind of preparation method of silver nanoparticle dendrite, which is characterized in that include the following steps:
A, copper rod is taken, is cleaned;The cleaning includes the following steps:Under Ultrasonic Conditions, use acetone, ethyl alcohol dilute successively Hydrochloric acid, distilled water clean copper rod;
B, silver nanoparticle dendrite is prepared, is included the following steps:
(1)Under room temperature, stirring condition, monovalence silver salt is taken to be dissolved in distilled water, obtains solution A;
(2)Copper rod obtained by step a is taken, solution A is added dropwise to copper rod, is reacted 20-80 seconds under normal temperature condition, uses distilled water flushing later Copper rod obtains the silver nanoparticle dendrite.
2. the preparation method of silver nanoparticle dendrite as described in claim 1, characterized in that the monovalence silver salt is AgNO3
3. the preparation method of silver nanoparticle dendrite as described in claim 1, characterized in that monovalence silver ion is dense in the solution A Degree is 0.05 M.
4. the preparation method of silver nanoparticle dendrite as described in claim 1, characterized in that anti-under the normal temperature condition in step b The time answered is 30-40 seconds.
CN201810684162.XA 2018-06-28 2018-06-28 A kind of preparation method of silver nanoparticle dendrite Withdrawn CN108723388A (en)

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Application Number Priority Date Filing Date Title
CN201810684162.XA CN108723388A (en) 2018-06-28 2018-06-28 A kind of preparation method of silver nanoparticle dendrite

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109848436A (en) * 2019-03-01 2019-06-07 淮海工学院 A method of preparing silver nanoparticle band

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109848436A (en) * 2019-03-01 2019-06-07 淮海工学院 A method of preparing silver nanoparticle band

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