CN108127126A - A kind of preparation and its application of thin slice leaf shape structure nano Cu - Google Patents
A kind of preparation and its application of thin slice leaf shape structure nano Cu Download PDFInfo
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- CN108127126A CN108127126A CN201711428837.6A CN201711428837A CN108127126A CN 108127126 A CN108127126 A CN 108127126A CN 201711428837 A CN201711428837 A CN 201711428837A CN 108127126 A CN108127126 A CN 108127126A
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- leaf shape
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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
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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
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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
- B22F1/0551—Flake form nanoparticles
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- Condensed Matter Physics & Semiconductors (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparations and its application of thin slice leaf shape structure nano Cu, belong to nano material preparation and application field.The preparation method is：Using copper sulphate as primary raw material; suitable catalyst, reducing agent and protective agent are added, 20~40min of magnetic agitation at 40~50 DEG C, suspension is centrifuged and is washed with deionized 3~5 times; it air-dries at room temperature, obtains ideal nanometer Cu thin slices leaf shape structure.There is radially superposed trend between the copper nano flake, form a string leaf shape, the conductive ink of high concentration can be prepared with good water solubility using it, so as to achieve the purpose that improve the Cu nano flake electrode material conductive capabilities being printed as.Compared with existing nano silver wire conductive ink, nanometer Cu thin slices leaf shape structure powder and conductive ink prepared by the present invention, raw material is less expensive, preparation method is simpler, be easier to stable operation, yield is high, equipment requirement is low, financial cost is low, more environment-friendly.
Description
Technical field
The invention belongs to nano material preparation and application fields, and in particular to solwution method directly prepares a kind of nanometer of Cu thin slice
Leaf shape structure provides technical support for the materialized application of Nanometer Copper.
Background technology
With the development of the technologies such as 3D printing, artificial intelligence, photoelectricity and application market, only 2017 conductive marking ink cities
Field demand will be more than 1900 tons.Currently, conductive marking ink is mainly silver nanoparticle, graphene, copper nano-wire marking ink etc., such as
CN107135602A, CN106519804A and CN106700735A.Nano silver wire is received because of its raw material fancy price, synthesis silver
Experiment condition needed for rice noodles and the graphene conductive ink of high concentration is harsh.And copper compares silver-colored, relative low price, and its
Also there is excellent electric conductivity, the good replacer of electrode material can be used as.
Currently, solwution method requirement of experiment is simple, relative efficiency and receive favor, it is logical especially in terms of conductive marking ink
Variously-shaped and performance materials, such as flexible electrode can be prepared by crossing 3D printing, mainly there is nano silver wire thin electrode and Tong Na
Rice noodles thin electrode, and copper nano-wire is because of too short (about 10 μm of copper nano-wire length), too thick (diameter about 90nm) and copper nano-wire
The reasons such as reunion copper nano flake electric conductivity is caused to be not so good as silver nanoparticle thin slice.Because this slim-lined construction feature, nano wire
Between contact area very little, cause its print nano flake electrodes conduct resistance value it is larger.Therefore a kind of structure is found, it can both drop
Low conduction resistance value, can also save material reduces cost, such as flaky texture, and overlapping has selection well between thin slice
Property.
Invention content
In order to overcome the deficiencies of the prior art, the technical problem to be solved in the present invention is to provide a kind of thin slice leaf shape structures to receive
The preparation method of rice Cu, to have radially superposed trend between the copper nano flake, forms a string leaf shape, has using it
Good water solubility prepares the conductive ink of high concentration, and the Cu nano flakes electrode material being printed as conduction is improved so as to reach
The purpose of ability.
The present invention is achieved by the following technical programs.
Using copper sulphate as primary raw material, suitable catalyst, reducing agent and protective agent are added, magnetic force stirs at 40~50 DEG C
20~40min is mixed, suspension is centrifuged and is washed with deionized 3~5 times, air-dries at room temperature, obtains ideal nanometer Cu
Thin slice leaf shape structure.
The catalyst is potassium hydroxide, and dosage is 10~20mol% of copper source amount.
The reducing agent is hydrazine hydrate, and dosage is 110~130mol% of copper source amount.
The protective agent is PVP (molecular weight 5000), and dosage is 0.5~1mol% of copper source amount.
After reaction, for product by centrifuging, centrifugal rotational speed is preferably 5000~6000rpm.
Detergent selects one or both of deionized water and absolute ethyl alcohol, and solid product is washed 3~5 times, removal
Responseless residue etc. in product air-dries spare.
Thin slice leaf shape structure nano Cu prepared by the above method can be applied in high concentration conductive ink is prepared.
The composition of above-mentioned high concentration conductive ink is：45wt% thin slice leaf shape structure nano Cu, 45wt% dipropylene glycol
Methyl ether, 10wt% wetting dispersing agents.
The preparation of above-mentioned high concentration conductive ink：45wt% nanometer copper particles, 45wt% dipropylene glycol methyl ethers and 10wt%
The grindings of wetting dispersing agent Disperbyk 180 are stirred 30min, then extra wetting and dispersing is removed with dipropylene glycol methyl ether
Agent centrifuges to obtain highly concentrated nano copper foil leaf shape structural conductive ink.
Using highly concentrated nano copper foil leaf shape structural conductive ink and commercially available copper powder and micron conductive ink, pass through respectively
Silk-screen printing, which is printed upon on PET substrates, obtains Cu nanometers of equal area and micro flakes electrode, and measure its resistance.
Compared with prior art, the present invention has following technique effect：
1st, a kind of nanometer of Cu thin slice leaf shape structure powder is prepared, is first compared with existing copper nano-wire and graphene conductive ink,
With better water solubility, highly concentrated nano Cu thin slice leaf shape conductive inks can be prepared；
2nd, high concentration Cu nano flake inks, the copper nano-electrode printed and nano silver wire electricity are prepared using this research
Pole, Graphene electrodes, copper nano-wire electrode have lower resistance value；
3rd, compared with existing nano silver wire conductive ink, a kind of nanometer of Cu thin slices leaf shape structure powder and conductive ink are prepared
Water, raw material is less expensive, preparation method is simpler, be easier to stable operation, yield is high, equipment requirement is low, financial cost is low, environment
It is friendly.
Description of the drawings
Fig. 1 is the XRD spectra of thin slice leaf shape structure nano Cu powders prepared by the embodiment of the present invention 7；
As seen from the figure, it is Cubic copper nanocrystalline structure.
Fig. 2 is the scanning electron microscope spectrogram (amplification ratio of thin slice leaf shape structure nano Cu powders prepared by the embodiment of the present invention 7
Example 150K ×)；
As seen from the figure, laminar Cu nano-particles form tri-lobed, then are overlapped along blade radial, form chain leaf
String.
Specific embodiment
The present invention is described in detail, but the present invention is not limited to following embodiments below in conjunction with specific embodiment.
Embodiment 1
20g copper sulphate is weighed, is completely dissolved at a temperature of 45 DEG C in 100mL deionized waters, then successively adds in 0.56g
KOH, 5.39g hydrazine hydrate and 2.5g PVP, the magnetic agitation 30min under 150rpm, suspension 5000rpm are centrifuged, are used in combination
Deionized water and washing 3 times, room temperature air-dries.
Embodiment 2
20g copper sulphate is weighed, is completely dissolved at a temperature of 45 DEG C in 100mL deionized waters, then successively adds in 0.84g
KOH, 5.39g hydrazine hydrate and 2.5g PVP, the magnetic agitation 30min under 150rpm, suspension 5000rpm are centrifuged, are used in combination
Deionized water and washing 3 times, room temperature air-dries.
Embodiment 3
20g copper sulphate is weighed, is completely dissolved at a temperature of 40 DEG C in 100mL deionized waters, then successively adds in 1.12g
KOH, 5.88g hydrazine hydrate and 2.5g PVP, the magnetic agitation 30min under 150rpm, suspension 6000rpm are centrifuged, are used in combination
Deionized water and washing 3 times, room temperature air-dries.
Embodiment 4
20g copper sulphate is weighed, is completely dissolved at a temperature of 45 DEG C in 100mL deionized waters, then successively adds in 0.84g
KOH, 6.37g hydrazine hydrate and 5g PVP, the magnetic agitation 40min under 150rpm, suspension 6000rpm are centrifuged, and are spent
Ionized water and washing 3 times, room temperature air-dries.
Embodiment 5
20g copper sulphate is weighed, is completely dissolved at a temperature of 40 DEG C in 100mL deionized waters, then successively adds in 1.12g
KOH, 6.37g hydrazine hydrate and 5g PVP, the magnetic agitation 30min under 150rpm, suspension 6000rpm are centrifuged, and are spent
Ionized water and washing 5 times, room temperature air-dries.
Embodiment 6
20g copper sulphate is weighed, is completely dissolved at a temperature of 45 DEG C in 100mL deionized waters, then priority addition 1g KOH,
6g hydrazine hydrates and 3g PVP, the magnetic agitation 20min under 150rpm, suspension 5000rpm centrifuge, and with deionized water with
Washing 3 times, room temperature air-dries.
Embodiment 7
20g copper sulphate is weighed, is completely dissolved at a temperature of 45 DEG C in 100mL deionized waters, then successively adds in 0.84g
KOH, 5.88g hydrazine hydrate and 2.5g PVP, the magnetic agitation 30min under 150rpm, suspension 5000rpm are centrifuged, are used in combination
Deionized water and washing 3 times, room temperature air-dries.
Embodiment 8
7 copper nano-particle of embodiment and each 2.25g of commercially available Micron-Sized Copper Powders Coated are weighed respectively, are separately added into 2.25g dipropyls two
Alcohol methyl ether, 0.5g wetting dispersing agents Disperbyk 180 prepare copper nano-particle and copper micron size conductive ink, print respectively
40 × 0.5mm thin slices, and its resistance value is measured respectively：25 Ω (copper nanometer) and 14 Ω (copper micron).
Claims (4)
1. a kind of preparation method of thin slice leaf shape structure nano Cu, which is characterized in that using copper sulphate as primary raw material, addition is suitable
Catalyst, reducing agent and the protective agent of amount, 20~40min of magnetic agitation at 40~50 DEG C, suspension are centrifuged and are spent
Ion water washing 3~5 times air-dries at room temperature to obtain the final product；
The catalyst is potassium hydroxide, and dosage is 10~20mol% of copper sulphate；
The reducing agent is hydrazine hydrate, and dosage is 110~130mol% of copper sulphate；
The protective agent is PVP, and dosage is 0.5~1mol% of copper sulphate.
2. the preparation method of thin slice leaf shape structure nano Cu as described in claim 1, which is characterized in that the PVP molecules
Measure is 5000.
3. thin slice leaf shape structure nano Cu prepared by method as described in claim 1 answering in high concentration conductive ink is prepared
With.
4. applications of the thin slice leaf shape structure nano Cu as claimed in claim 3 in high concentration conductive ink is prepared, special
Sign is that the composition of the high concentration conductive ink is：45wt% thin slice leaf shape structure nano Cu, 45wt% dipropylene glycol first
Ether, 10wt% wetting dispersing agents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711428837.6A CN108127126A (en) | 2017-12-26 | 2017-12-26 | A kind of preparation and its application of thin slice leaf shape structure nano Cu |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711428837.6A CN108127126A (en) | 2017-12-26 | 2017-12-26 | A kind of preparation and its application of thin slice leaf shape structure nano Cu |
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| Publication Number | Publication Date |
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| CN108127126A true CN108127126A (en) | 2018-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711428837.6A Pending CN108127126A (en) | 2017-12-26 | 2017-12-26 | A kind of preparation and its application of thin slice leaf shape structure nano Cu |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| JP2008013837A (en) * | 2006-07-10 | 2008-01-24 | Sumitomo Metal Mining Co Ltd | Fine copper powder and its manufacturing method |
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2017
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| CN103658675A (en) * | 2013-12-23 | 2014-03-26 | 广东东硕科技有限公司 | Copper nanowire and preparation method thereof |
| CN103801709A (en) * | 2014-03-17 | 2014-05-21 | 中国科学院新疆理化技术研究所 | Synthetic method of copper nano-particles of different shapes |
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Non-Patent Citations (1)
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Cited By (1)
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| 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 |
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Application publication date: 20180608 |