CN107398561A - A kind of preparation method of the copper nanometer sheet with regular shape - Google Patents
A kind of preparation method of the copper nanometer sheet with regular shape Download PDFInfo
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- CN107398561A CN107398561A CN201710511086.8A CN201710511086A CN107398561A CN 107398561 A CN107398561 A CN 107398561A CN 201710511086 A CN201710511086 A CN 201710511086A CN 107398561 A CN107398561 A CN 107398561A
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- copper
- nanometer sheet
- preparation
- steel plate
- regular shape
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Classifications
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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
- 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
-
- 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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
Abstract
The invention discloses a kind of preparation method of the copper nanometer sheet with regular shape, solves the problems, such as that the copper nanometer sheet that existing preparation method obtains is in irregular shape.Concretely comprise the following steps（1）Solvent is heated to 30 90 DEG C, water-soluble mantoquita is added under stirring condition, deposition solution is obtained after being completely dissolved；（2）Steel plate is immersed in above-mentioned deposition solution, rinsed the deposition layer surface on steel plate with absolute ethyl alcohol well after placing 5 120 minutes, and be dried at room temperature for；（3）The copper nano-precipitation layer obtained on steel plate is scraped to collect and produced.Obtained copper nanometer sheet has well-regulated hexagonal flake and seldom surface defect, and is not in adhesion and to develop into the phenomenon of bulk druse between crystal.The material has significant value on as the material such as polymer coating anticorrosive packing and excellent conductive and heat-conductive, catalysis.
Description
Technical field
The present invention relates to field of nano material preparation, and in particular to a kind of preparation method of copper nanometer sheet.
Background technology
As a kind of more important functional material, copper metal because its superior performance, small toxicity, it is cheap the advantages that
It is widely applied in industrial production, daily life, and exists relative to the bigger copper product of micron order or particle diameter, copper nanocrystallite
Electrical and thermal conductivity performance, electro-chemical activity, catalytic performance etc. possess more prominent performance, thus can obtain scientific research and
Production field is widely paid close attention to.
Because copper has typical face-centered cubic crystal formation, it, which has, significantly tends to three-dimensional solid matter and is grown to serve as three dimensional particles
Characteristic, thus allow it controllably to grow into flake nano material according to two-dimensional directional there is very big difficulty.Patent CN
103170647 B disclose the method that liquid-phase reduction means prepare copper nanometer sheet, but the method is disadvantageous in that, by being obtained
The copper nanometer sheet crystal obtained is to be obtained by initially smaller three-dimensional copper nano particles by way of self assembly, is ultimately generated
Flat crystal shows extremely irregular shape, or even lamella is bent.And the copper nanometer sheet with regular shape
Quality is higher, so preparing the copper nanometer sheet with regular shape turns into problem to be captured.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided a kind of preparation of the copper nanometer sheet with regular shape
Method.
For achieving the above object, the technical solution adopted in the present invention is：A kind of copper nanometer with regular shape
The preparation method of piece, the method includes the steps of：
（1）Solvent is heated to 30-90 DEG C, the mass ratio of water-soluble mantoquita, mantoquita and solvent is added under the conditions of magnetic agitation
For 1:15-40, deposition solution is obtained after being completely dissolved；
（2）Immersed steel plate as substrate in above-mentioned deposition solution, maintain the deposition solution in certain temperature, placement 5-120
The deposition layer surface on steel plate is rinsed well with absolute ethyl alcohol after minute, and is dried at room temperature for；
（3）The copper nano-precipitation layer obtained on steel plate is scraped to collect and produced.
Above-mentioned steps（1）In, solvent used is distilled water, ethylene glycol, glycerine, polyethylene glycol 200, polyethylene glycol
400 or Macrogol 600 in one kind.
Above-mentioned steps（1）In, water-soluble mantoquita used is one kind in copper nitrate, copper chloride, copper sulphate.
Above-mentioned steps（2）In, steel plate material used is one kind in 304L, 316L or Q235B.
Above-mentioned steps（2）In, the maintenance temperature of deposition solution is any temperature in 30-120 DEG C in deposition process.
In the method disclosed in this patent, we are prepared for the copper nanometer sheet of high-quality using replacement deposition technology.This
One technology has reduction sex differernce and the characteristic of replacement deposition reaction occurs between utilizing metallic element, in relatively low reaction temperature and
Copper nanocrystallite sedimentary can be obtained under atmospheric pressure environment in base steel plate surface, while there is the work of template by solvent itself
With the nano-sheet that crystal can be in strict accordance with two-dimentional pattern growth into rule.The sedimentary of acquisition has loose, structural strength
The characteristics of very low, thus it is that can obtain scattered copper nanometer sheet powder to peel off mode by simple physics.Examined through SEM photograph
Survey, obtain two-dimensional slice nano material and have well-regulated six sides shape and seldom surface defect, and be not in viscous between crystal
Connect and develop into the phenomenon of bulk druse.The material is as polymer coating anticorrosive packing and excellent conductive and heat-conductive, catalysis
Deng having significant value on material.
The beneficial effect of this method is：Preparation process step is simple, is put into without high energy consumption, obtains flaky nanocrystalline purity
Height, and change of the dimensional parameters of obtained copper nanometer sheet to technological parameters such as reaction raw materials concentration, temperature of reaction system is insensitive.
Importantly, obtaining two-dimentional copper nanometer sheet has regular shape and seldom surface defect.The material is as excellent conductive
There is significant value in terms of the materials such as heat conduction, electrochemical sensing and catalysis.
Brief description of the drawings
Figure 1A is the SEM photograph (1 μm) of the copper nanometer sheet sedimentary prepared in embodiment 3 on Q235B substrates.
Figure 1B is the SEM photograph (500nm) of the copper nanometer sheet sedimentary prepared in embodiment 3 on Q235B substrates.
Fig. 2 is the XRD spectra for the product that embodiment 3 obtains.
Fig. 3 is the SEM photograph that the product that embodiment 3 obtains is dispersed through rear single copper nanometer sheet crystal.
Fig. 4 is that the copper nanometer sheet that will be collected in embodiment 6 is distributed to E44 type epoxy resin with different quality percentage and obtained
The different Tafel polarization curves showed after coating.
Embodiment
The following examples are that the present invention is described in further detail：
Embodiment 1：
（1）40 DEG C are heated to using 50 mL distilled water as solvent, 2.50 g copper nitrates are slowly added under the conditions of magnetic agitation,
The mass ratio of copper nitrate and distilled water is 1:20, obtain deposition solution after being completely dissolved；
（2）Using 304L steel plates as substrate, steel plate is washed after the polishing of 400,800 and 1000 mesh carborundum papers through distillation successively
Only and dry, be subsequently dipped in above-mentioned deposition solution, maintain temperature that the copper nanometer on steel plate is sunk after placing 10 minutes at 45 DEG C
Build-up surface is fully rinsed with absolute ethyl alcohol, is then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with scraper, obtains product of the present invention, this product can be utilized directly.
Embodiment 2：
（1）60 DEG C are heated to using 50 mL glycerine as solvent, 1.63 g copper nitrates are slowly added under the conditions of magnetic agitation,
The mass ratio of copper nitrate and glycerine is 1:40, obtain deposition solution after being completely dissolved；
（2）It will clean and dry through distilled water after the processing of 304L steel plate sandblastings, be subsequently dipped in above-mentioned deposition solution, maintain temperature
At 55 DEG C, place 15 minutes；The deposition layer surface obtained on copper coin is fully rinsed with absolute ethyl alcohol after the completion of deposition reaction, with
After be dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with blade, obtains product of the present invention, this product can be utilized directly.
Embodiment 3：
（1）60 DEG C are heated to using 50 mL polyethylene glycol 400s as solvent, 2.04 g chlorine are slowly added under the conditions of magnetic agitation
The mass ratio of change copper, copper chloride and polyethylene glycol 400 is 1:27, obtain deposition solution after being completely dissolved；
（2）Using Q235B steel plates as substrate, steel plate is successively through distilled water after the polishing of 400,800 and 1000 mesh carborundum papers
Clean and dry, be subsequently dipped in above-mentioned deposition solution, maintain temperature to be placed 20 minutes at 60 DEG C；Will after the completion of deposition reaction
The deposition layer surface of acquisition is fully rinsed with absolute ethyl alcohol, is then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with scraper, obtains product of the present invention.
Figure 1A and Figure 1B is the SEM photograph for the sedimentary that the present embodiment is prepared on Q235B substrates, can be sent out from the figure
Existing, the layers of copper of deposition is in typical multilevel hierarchy, and construction unit is made up of two-dimentional copper nanometer sheet.Fig. 2 XRD spectra, passes through
By the diffraction maximum detected and standard spectrogram（JADE PDF-2 Card）It is corresponding, it is found that copper simple substance only occurs in sedimentary
Crystal diffraction peak, it can be verified that the copper deposits obtained are the simple substance copper crystal of high-purity.
Fig. 3 is the SEM that the single crystal shot after obtained copper nanometer sheet powder high degree of dispersion will be collected in the present embodiment
Photo, from the figure it can be found that crystal shows regular hexagon or pentagonal configuration, and surface does not have defect substantially.
Embodiment 4：
（1）90 DEG C are heated to using 50 mL glycerine as solvent, 2.17 g copper chlorides, copper are slowly added under the conditions of magnetic agitation
The mass ratio of salt and solvent is 1:30, obtain deposition solution after being completely dissolved；
（2）Cleaned simultaneously through distilled water after the polishing of 400,800 and 1000 mesh carborundum papers successively using Q235B steel plates as substrate
Drying, is subsequently dipped in above-mentioned deposition solution, maintains temperature to be placed 5 minutes at 110 DEG C；By acquisition after the completion of deposition reaction
Deposition layer surface is fully rinsed with absolute ethyl alcohol, is then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with scraper, obtains product of the present invention.
Embodiment 5：
（1）55 DEG C are heated to using 50 mL distilled water as solvent, 2.50 g copper sulphate, copper are slowly added under the conditions of magnetic agitation
The mass ratio of salt and solvent is 1:25, obtain deposition solution after being completely dissolved；
（2）Cleaned simultaneously through distilled water after the polishing of 400,800 and 1000 mesh carborundum papers successively using Q235B steel plates as substrate
Drying, is subsequently dipped in above-mentioned deposition solution, maintains temperature to be placed 15 minutes at 40 DEG C；By acquisition after the completion of deposition reaction
Deposition layer surface is fully rinsed with absolute ethyl alcohol, is then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with scraper, obtains product of the present invention.
Embodiment 6：
（1）60 DEG C are heated to using 50 mL polyethylene glycol 400s as solvent, 4.20 g chlorinations are slowly added under the conditions of magnetic agitation
The mass ratio of copper, mantoquita and solvent is 1:15, obtain deposition solution after being completely dissolved；
（2）Cleaned simultaneously through distilled water after the polishing of 400,800 and 1000 mesh carborundum papers successively using 304L steel plates as substrate
Drying, is subsequently dipped in above-mentioned deposition solution, maintains temperature to be placed 100 minutes at 80 DEG C；By acquisition after the completion of deposition reaction
Deposition layer surface is fully rinsed with absolute ethyl alcohol, is then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with blade, obtains product of the present invention.
Different content is taken to be added to 2 g at room temperature into the E44 types of liquid respectively the copper nanometer sheet collected in the embodiment
Turn into mixed system in epoxy resin, 0.055 g ethylenediamines are then added dropwise into the blend and 0.032 g Tween 80s are made respectively
For curing agent and levelling agent, the min of mechanical agitation 15 it is to be mixed uniformly after after hybrid resin is coated on Q235B steel plates；Then
The steel plate for being coated with semi-solid resin coating is transferred in drying box and solidifies 10 h at 80 DEG C, that is, obtains containing different fillers hundred
Divide ratio（0,0.47,1.42 and 2.38 wt %）Epoxy coating.These coating samples are placed in three-electrode system, point
Not using coating sample, platinum electrode and saturated calomel electrode as working electrode, to electrode and reference electrode, with alkaline solution of NaCl
（Containing 3.5 wt % NaCl and 2 wt % NaOH）As corrosive electrolyte, the Tafel polarization curves of each coating have been obtained,
As shown in Figure 4.It can be seen that compared to pure epoxy coating, with filler than increasing, it corrodes the coating of cupric nanometer sheet filler
Current potential（E corr ）Constantly shuffle, and corrosion electric current density（i corr ）Constantly reduce, this has absolutely proved that epoxy coating is being filled
Antisepsis strengthens after the copper nanometer sheet powder, that is, confirms application value of the copper nanometer sheet in corrosion-resistant field.
Embodiment 7：
（1）60 DEG C are heated to using 50 mL Macrogol 600s as solvent, 1.53 g chlorinations are slowly added under the conditions of magnetic agitation
The mass ratio of copper, mantoquita and solvent is 1:35, obtain deposition solution after being completely dissolved；
（2）Clean and dry through distilled water after blasting treatment successively using Q235B steel plates as substrate, be subsequently dipped to above-mentioned deposition
In solution, temperature is maintained to be placed 40 minutes at 80 DEG C；The deposition layer surface of acquisition is filled with absolute ethyl alcohol after the completion of deposition reaction
Divide and rinse, be then dried at room temperature for；
（3）The copper nano-precipitation layer of acquisition is scraped into collection with blade, obtains product of the present invention.
Claims (5)
- A kind of 1. preparation method of the copper nanometer sheet with regular shape, it is characterised in that：Specifically comprise the steps of：（1）Solvent is heated to 30-90 DEG C, the mass ratio of water-soluble mantoquita, mantoquita and solvent is added under the conditions of magnetic agitation For 1:15-40, deposition solution is obtained after being completely dissolved；（2）Immersed steel plate as substrate in above-mentioned deposition solution, maintain the deposition solution in certain temperature, placement 5-120 The deposition layer surface on steel plate is rinsed well with absolute ethyl alcohol after minute, and is dried at room temperature for；（3）The copper nano-precipitation layer obtained on steel plate is scraped to collect and produced.
- 2. the preparation method of the copper nanometer sheet according to claim 1 with regular shape, it is characterised in that：The step （1）In, solvent used is in distilled water, ethylene glycol, glycerine, polyethylene glycol 200, polyethylene glycol 400 or Macrogol 600 One kind.
- 3. the preparation method of the copper nanometer sheet according to claim 1 with regular shape, it is characterised in that：The step （1）In, water-soluble mantoquita used is one kind in copper nitrate, copper chloride, copper sulphate.
- 4. the preparation method of the copper nanometer sheet according to claim 1 with regular shape, it is characterised in that：The step （2）In, steel plate material used is one kind in 304L, 316L or Q235B.
- 5. the preparation method of the copper nanometer sheet according to claim 1 with regular shape, it is characterised in that：The step （2）In, the maintenance temperature of deposition solution is any temperature in 30-120 DEG C in deposition process.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067254A (en) * | 2017-12-21 | 2018-05-25 | 苏州大学 | The preparation method of copper oxide nanocrystal and silver/copper oxide heterojunction structure |
| CN109663932A (en) * | 2018-03-16 | 2019-04-23 | 南京林业大学 | A kind of preparation method of flake silver powder |
| CN109877336A (en) * | 2018-03-16 | 2019-06-14 | 南京林业大学 | A kind of preparation method of flake copper powder |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN111468740A (en) * | 2020-04-07 | 2020-07-31 | 延边大学 | Method for preparing hexagonal elemental copper nanosheet by using polyol method |
| CN113500202A (en) * | 2021-07-14 | 2021-10-15 | 哈尔滨理工大学 | Preparation method of high-purity hexagonal Cu nanocrystalline |
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| CN101987359A (en) * | 2010-11-16 | 2011-03-23 | 蒋剑秋 | Preparation method of reduced copper coated iron composite powder by using wet method |
| CN103191740A (en) * | 2013-03-18 | 2013-07-10 | 环境保护部华南环境科学研究所 | Copper-sponge iron bimetallic catalyst as well as preparation method and application thereof |
| CN104016313A (en) * | 2014-06-10 | 2014-09-03 | 郑州轻工业学院 | Preparation method of hexagonal copper selenide nanosheets |
| CN105297081A (en) * | 2015-11-13 | 2016-02-03 | 武汉大学 | Method for preparing two-dimensional lamellar copper nanometer piece through electrochemistry |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101987359A (en) * | 2010-11-16 | 2011-03-23 | 蒋剑秋 | Preparation method of reduced copper coated iron composite powder by using wet method |
| CN103191740A (en) * | 2013-03-18 | 2013-07-10 | 环境保护部华南环境科学研究所 | Copper-sponge iron bimetallic catalyst as well as preparation method and application thereof |
| CN104016313A (en) * | 2014-06-10 | 2014-09-03 | 郑州轻工业学院 | Preparation method of hexagonal copper selenide nanosheets |
| CN105297081A (en) * | 2015-11-13 | 2016-02-03 | 武汉大学 | Method for preparing two-dimensional lamellar copper nanometer piece through electrochemistry |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108067254A (en) * | 2017-12-21 | 2018-05-25 | 苏州大学 | The preparation method of copper oxide nanocrystal and silver/copper oxide heterojunction structure |
| CN109663932A (en) * | 2018-03-16 | 2019-04-23 | 南京林业大学 | A kind of preparation method of flake silver powder |
| CN109877336A (en) * | 2018-03-16 | 2019-06-14 | 南京林业大学 | A kind of preparation method of flake copper powder |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN111468740A (en) * | 2020-04-07 | 2020-07-31 | 延边大学 | Method for preparing hexagonal elemental copper nanosheet by using polyol method |
| CN113500202A (en) * | 2021-07-14 | 2021-10-15 | 哈尔滨理工大学 | Preparation method of high-purity hexagonal Cu nanocrystalline |
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Application publication date: 20171128 |