CN105562675A - Preparation method of nitric acid induced gold nanobelt - Google Patents

Preparation method of nitric acid induced gold nanobelt Download PDF

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Publication number
CN105562675A
CN105562675A CN201510897529.2A CN201510897529A CN105562675A CN 105562675 A CN105562675 A CN 105562675A CN 201510897529 A CN201510897529 A CN 201510897529A CN 105562675 A CN105562675 A CN 105562675A
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China
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solution
nitric acid
preparation
nanobelt
gold nano
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CN201510897529.2A
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Chinese (zh)
Inventor
王耀斌
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Shaanxi Shengmai Petroleum Co Ltd
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Shaanxi Shengmai Petroleum Co Ltd
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Priority to CN201510897529.2A priority Critical patent/CN105562675A/en
Publication of CN105562675A publication Critical patent/CN105562675A/en
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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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/068Flake-like particles
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to the technical field of preparation of rare metal materials, in particular to a preparation method of a nitric acid induced gold nanobelt by a seeding method. The preparation method of the nitric acid induced gold nanobelt comprises the steps of adding a trisodium citrate solution to a 3-neck flask and heating; injecting a chloroauric acid solution while stirring; finally turning the solution into wine red, removing a heat source, stopping stirring, cooling and keeping in dark place at 4 DEG C; dissolving CTAB (Cetyl Trimethyl Ammonium Bromide) and heating in water bath; injecting 830 uL of HAuCl4 solution, a nitric acid solution and an ascorbic acid solution; injecting a gold sol until the solution turns into dark red and red brown, cooling to room temperature, centrifugal separating, discarding a supernatant liquid and clarifying the solution to obtain the nitric acid induced gold nanobelt. A single-crystal gold nanobelt prepared by using the seeding method has a width between 50 nm and 200 nm and a length between 0.7 pm and 3 pm; the nanobelt is smooth and complete in surface, good in crystallinity and grows along the 111 crystal orientation; the method provided by the invention is simple and easy to operate, high in operability and liable to popularization and utilization in large area.

Description

A kind of preparation method of nitric acid induction gold nano band
Technical field
The present invention relates to Rare Metals Materials preparing technical field, be specifically related to the crystal seed method preparation method of a kind of nitric acid induction gold nano band.
Background technology
Nanobelt is a kind of one-dimensional nano structure of latest report after nano wire and nanotube.Since having prepared zinc oxide nano-belt first, nanobelt has been subject to extensive concern because it is different from pipe, the novel structure of wire material and the photoelectric properties of uniqueness.The two ends of gold nano band have strong enhancing electric field, different plasma bands of a spectrum are demonstrated in long axis direction and minor axis cross-directional, very responsive to the dielectric constant of surrounding medium, this characteristic electron makes it get a good chance of becoming a kind of nano material obtaining important application in nanophotonics, sensory field.
At present, there is " family " phenomenon in the research work of nanobelt, concentrates on the VI race semi-conducting materials such as oxide, sulfide, selenides.Especially the preparation of oxide nanobelts and character research, comparative maturity.But the synthesis of metal nanobelt report is less, particularly has the gold of high symmetry face-centred cubic structure.With the minimum spherical particle of surface energy for Main Morphology, the preparation of anisotropy gold nano band still has larger challenge.At present, the method that people synthesize gold nano-material mainly contains reducing process, crystal seed method, microemulsion method etc., obtain product form except size controlled
Nanometer rods and spherical particle outside, also obtain the gold nano grain of the various profiles such as hexagon sheet, cube and star.The acquisition of gold nano band adopts sonochemistry method to complete recently, but how to adopt the simplest system to prepare gold nano band still to have important theory and realistic meaning.
Summary of the invention
The present invention is intended to propose a kind of method utilizing the simplest system to prepare gold nano band.
Technical program of the present invention lies in:
A preparation method for nitric acid induction gold nano band, adopts following steps:
3mL citric acid three sodium solution is joined in the there-necked flask filling the 100mL aqueous solution, is heated to boiling; Chlorauric acid solution is injected under stirring; Regulate thermal source to make reaction system keep micro-ly boiling, stir, solution from light yellowly becoming colourless, grey, finally become claret, remove thermal source, stop stirring, be cooled to room temperature, keep in Dark Place in 4 DEG C;
1.71gCTAB being dissolved into 20mL tri-boils off in ionized water, heating water bath; Get 830 μ LHAuCl 4solution injects flask, and solution presents orange red; Reinject salpeter solution and 200 μ L ascorbic acid solutions; The aurosol of 200 μ L is injected within 1min, solution colour first by orange red change into colourless, present pink, redness gradually again, until peony and bronzing, be cooled to room temperature, centrifugation after reaction 2h, discard upper strata settled solution, the precipitation obtained is scattered in suitable quantity of water solution again, obtains nitric acid induction gold nano band.
Preferably, the described CTAB/HAuCl added 4solution proportion is 235:1.
Preferably, the speed of described centrifugation is 5000r/min.
Preferably, the concentration of the described chlorauric acid solution added is 0.024mol/L, and the amount added is 1mL.
Or the temperature of preferably, described heating water bath is 50 DEG C.
Or preferably, used in described reaction raw material is: the concentration of citric acid three sodium solution 0.034mol/L, HAuCl4 is 0.024mol/L, ascorbic acid solution 0.2mol/L, salpeter solution 1mol/L.
Technique effect of the present invention is:
The present invention adopts crystal seed method to prepare monocrystalline gold nano band, width between 50 ~ 200nm, length be 0.7 ~ 3pm not etc.The surface smoothing of nanobelt is complete, and crystallinity is good, and along 111 crystal orientation growths.And method provided by the invention is simple, operability is high, is easy to spread and uses.
Detailed description of the invention
A preparation method for nitric acid induction gold nano band, adopts following steps:
3mL citric acid three sodium solution is joined in the there-necked flask filling the 100mL aqueous solution, is heated to boiling; Chlorauric acid solution is injected under stirring; Regulate thermal source to make reaction system keep micro-ly boiling, stir, solution from light yellowly becoming colourless, grey, finally become claret, remove thermal source, stop stirring, be cooled to room temperature, keep in Dark Place in 4 DEG C;
1.71gCTAB being dissolved into 20mL tri-boils off in ionized water, heating water bath; Get 830 μ LHAuCl 4solution injects flask, and solution presents orange red; Reinject salpeter solution and 200 μ L ascorbic acid solutions; The aurosol of 200 μ L is injected within 1min, solution colour first by orange red change into colourless, present pink, redness gradually again, until peony and bronzing, be cooled to room temperature, centrifugation after reaction 2h, discard upper strata settled solution, the precipitation obtained is scattered in suitable quantity of water solution again, obtains nitric acid induction gold nano band.
Wherein, the CTAB/HAuCl added 4solution proportion is 235:1.The speed of centrifugation is 5000r/min.The concentration of the chlorauric acid solution added is 0.024mol/L, and the amount added is 1mL.The temperature of heating water bath is 50 DEG C.Raw material used in reaction is: the concentration of citric acid three sodium solution 0.034mol/L, HAuCl4 is 0.024mol/L, ascorbic acid solution 0.2mol/L, salpeter solution 1mol/L.

Claims (6)

1. it is characterized in that: adopt following steps:
3mL citric acid three sodium solution is joined in the there-necked flask filling the 100mL aqueous solution, is heated to boiling; Chlorauric acid solution is injected under stirring; Regulate thermal source to make reaction system keep micro-ly boiling, stir, solution from light yellowly becoming colourless, grey, finally become claret, remove thermal source, stop stirring, be cooled to room temperature, keep in Dark Place in 4 DEG C;
1.71gCTAB being dissolved into 20mL tri-boils off in ionized water, heating water bath; Get 830 μ LHAuCl 4solution injects flask, and solution presents orange red; Reinject salpeter solution and 200 μ L ascorbic acid solutions; The aurosol of 200 μ L is injected within 1min, solution colour first by orange red change into colourless, present pink, redness gradually again, until peony and bronzing, be cooled to room temperature, centrifugation after reaction 2h, discard upper strata settled solution, the precipitation obtained is scattered in suitable quantity of water solution again, obtains nitric acid induction gold nano band.
2., as the preparation method of a claim 1 nitric acid induction gold nano band, it is characterized in that: the described CTAB/HAuCl added 4solution proportion is 235:1.
3., as the preparation method of a claim 1 nitric acid induction gold nano band, it is characterized in that: the speed of described centrifugation is 5000r/min.
4., as the preparation method of a claim 1 nitric acid induction gold nano band, it is characterized in that: the concentration of the described chlorauric acid solution added is 0.024mol/L, the amount added is 1mL.
5., as the preparation method of a claim 1 nitric acid induction gold nano band, it is characterized in that: the temperature of described heating water bath is 50 DEG C.
6. as the preparation method of a claim 1 nitric acid induction gold nano band, it is characterized in that: raw material used in described reaction is: citric acid three sodium solution 0.034mol/L, the concentration of HAuCl4 is 0.024mol/L, ascorbic acid solution 0.2mol/L, salpeter solution 1mol/L.
CN201510897529.2A 2015-12-08 2015-12-08 Preparation method of nitric acid induced gold nanobelt Pending CN105562675A (en)

Priority Applications (1)

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CN201510897529.2A CN105562675A (en) 2015-12-08 2015-12-08 Preparation method of nitric acid induced gold nanobelt

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Application Number Priority Date Filing Date Title
CN201510897529.2A CN105562675A (en) 2015-12-08 2015-12-08 Preparation method of nitric acid induced gold nanobelt

Publications (1)

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CN105562675A true CN105562675A (en) 2016-05-11

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108247039A (en) * 2018-03-06 2018-07-06 上海应用技术大学 A kind of preparation method of gold nano band
CN108918855A (en) * 2018-07-31 2018-11-30 济南大学 A kind of preparation method and application based on signal " on-off " type Electrochemiluminescsensor sensor that AgNCs is illuminator

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108247039A (en) * 2018-03-06 2018-07-06 上海应用技术大学 A kind of preparation method of gold nano band
CN108918855A (en) * 2018-07-31 2018-11-30 济南大学 A kind of preparation method and application based on signal " on-off " type Electrochemiluminescsensor sensor that AgNCs is illuminator
CN108918855B (en) * 2018-07-31 2021-11-09 济南大学 Preparation method and application of signal 'on-off' type electrochemiluminescence sensor based on AgNCs as luminophor

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Application publication date: 20160511