CN110026567A - Silver-copper nano particle and its preparation method and application - Google Patents
Silver-copper nano particle and its preparation method and application Download PDFInfo
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- CN110026567A CN110026567A CN201910332310.6A CN201910332310A CN110026567A CN 110026567 A CN110026567 A CN 110026567A CN 201910332310 A CN201910332310 A CN 201910332310A CN 110026567 A CN110026567 A CN 110026567A
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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
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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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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Abstract
The present invention relates to a kind of silver-copper nano particles and its preparation method and application.The preparation method comprises the following steps: nonpolar solvent being heated to 100 DEG C -150 DEG C, then mantoquita, silver salt, fatty acid, fatty amine and reducing agent are added into the nonpolar solvent, obtains mixture for heat preservation;The mixture is heated to 180 DEG C -300 DEG C, cooling after 1h-3h is stirred, alcohols solvent is added, must precipitate, as silver-copper nano particle;The nonpolar solvent is selected from saturation or unsaturated alkane.This method utilizes the principle of coreduction synthesis, silver-copper nano particle has successfully been made, wherein the ratio of silver-bearing copper is controllable, easy to operate, the easy volume production of technique.
Description
Technical field
The present invention relates to ink-jet printing fields, more particularly to silver-copper nano particle and its preparation method and application.
Background technique
Ink-jet printing process is widely used in manufacture conductor wire.This method has at low cost, implements simple, environmental protection etc. is many
Advantage.Electrically conductive ink generally includes silver, copper, nickel, tin etc..Main selection silver nano-grain because they have high conductivity and
Excellent inoxidizability.However, the high price of silver is its critical defect for being used as electrically conductive ink, while silver is easy to go out because of potential difference
Existing electron transition phenomenon, leads to short circuit.Copper has low-down cost and relatively high electric conductivity, and is becoming and most inhaling
The substitution metal of gravitation.
However copper is highly unstable in air, and is easily oxidised.So proposing that one kind is received for enhancing copper at present
The method of rice grain stability is that copper and other metal bondings are formed duplex metal nano granule, the i.e. nanometer of nucleocapsid result
Grain.A kind of generation nucleocapsid knot that production core-shell structure is replaced to prevent copper nano particles from aoxidizing by galvanic couple has been disclosed at present
The nanoparticle approach of structure.However, this method usually requires the program of two separation to be respectively synthesized core and shell, and it is difficult to control
The growth of outer cover metal processed, often will lead to shell growth it is too fast, lead to the proportional imbalance between two kinds of metals.
Summary of the invention
Based on this, the present invention provides a kind of preparation method of silver-copper nano particle, and this method utilizes the original of coreduction synthesis
Reason, has successfully been made silver-copper nano particle, wherein the ratio of silver-bearing copper is controllable, easy to operate, the easy volume production of technique, using this method
Silver-copper nano particle obtained can prevent copper to be oxidized and reduce the cost, and improve electric conductivity.
The specific technical proposal is:
A kind of preparation method of silver-copper nano particle, comprising the following steps:
Nonpolar solvent is heated to 100 DEG C -150 DEG C, then mantoquita, silver is added in heat preservation into the nonpolar solvent
Salt, fatty acid, fatty amine and reducing agent, obtain mixture;
The mixture is heated to 180 DEG C -300 DEG C, cooling after 1h-3h is stirred, alcohols solvent is added, must precipitate, i.e.,
For silver-copper nano particle;
The nonpolar solvent is selected from saturation or unsaturated alkane.
The nonpolar solvent is selected from the tetradecane or 1- octadecylene in one of the embodiments,.
The molar ratio of the metal salt, fatty acid, fatty amine and reducing agent is 5:(4- in one of the embodiments,
10): (4-10): (4-10), the molal quantity of the metal salt are the sum of the mantoquita and the molal quantity of silver salt.
In one of the embodiments, in nonpolar solvent described in 1L, the metal salt of 10mmol-15mmol is added.
The mantoquita is selected from copper acetate in one of the embodiments,.
The silver salt is selected from silver acetate in one of the embodiments,.
The fatty acid is selected from C12-C22 saturation or unsaturated fatty acid in one of the embodiments,.
The fatty acid is selected from stearic acid, palmitinic acid, myristic acid, lauric acid and oleic acid in one of the embodiments,
One or more of.
The fatty amine is selected from C16-C18 saturation or unsaturated fat amine in one of the embodiments,.
The fatty amine is oleyl amine in one of the embodiments,.
The reducing agent is in 1- octadecanol, oleyl alcohol and 1,2- hexadecane diol in one of the embodiments,
It is one or more of.
It is in one of the embodiments, ethyl alcohol to the alcohols solvent.
The present invention also provides a kind of silver-copper nano particles.
The specific technical proposal is:
A kind of silver-copper nano particle, is made by above-mentioned preparation method.
The present invention also provides a kind of inks.
The specific technical proposal is:
A kind of ink, raw material include above-mentioned silver-copper nano particle.
Compared with prior art, the invention has the following advantages:
The preparation method of silver-copper nano particle of the present invention first dissolves silver salt, mantoquita, rouge in hot nonpolar solvent
Fat acid, fatty amine and reducing agent, obtain mixture, then, increase the temperature of mixture, and after keeping the temperature a period of time, silver-bearing copper is made
Nano particle.Wherein, hot nonpolar solvent its can prevent nanoparticle aggregate, be conducive to silver salt and mantoquita in fatty acid and
It is dissociated in fatty amine, is conducive to the progress of coreduction reaction.Meanwhile relative to the silver-copper nano particle for preparing core-shell structure, on
The ratio of silver-bearing copper in final silver-copper nano particle can be controlled by adjusting the additional amount of silver salt and mantoquita by stating preparation method, will not
Lead to the proportional imbalance between two kinds of metals, and technological operation is simple, easy volume production.Final silver-copper nano particle obtained can
It prevents copper to be oxidized, and can reduce the cost, improve electric conductivity.
Wherein, when preparing silver-copper nano particle, preferred nonpolar solvent is the tetradecane, and the tetradecane under high temperature is more sharp
It is dissociated in fatty acid and fatty amine in silver salt and mantoquita, promotes the progress of coreduction reaction, effectively prevent silver-copper nano particle
Reunite.
Detailed description of the invention
Fig. 1 is the XRD diagram of the silver-copper nano particle of embodiment 1;
Fig. 2 is the TEM figure of the silver-copper nano particle of embodiment 1;
Fig. 3 is the XRD diagram of the silver-copper nano particle of embodiment 2;
Fig. 4 is the TEM figure of the silver-copper nano particle of embodiment 2.
Specific embodiment
Silver-copper nano particle of the invention and its preparation method and application is made below in conjunction with specific embodiment further detailed
Thin explanation.The invention can be realized in many different forms, however it is not limited to embodiments described herein.On the contrary
Ground, the purpose of providing these embodiments is that making to understand the disclosure of invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
Embodiment 1
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, the tetradecane is heated to 130 DEG C, 30min is kept the temperature, is then added into the tetradecane of 0.2L
The copper acetate of 2mmol, the silver acetate of 0.5mmol, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol 1,2- hexadecane diol,
Obtain mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
X-ray diffraction (XRD) figure of silver-copper nano particle obtained by the present embodiment as shown in Figure 1, transmission electron microscope (TEM) figure such as
Shown in Fig. 2.
XRD spectrum is shown, containing silver and copper in particle made from the present embodiment, illustrates that the present embodiment is successfully prepared silver-bearing copper
Nano particle, TEM map show that silver-copper nano grain diameter is uniform, do not reunite.
Using above-mentioned silver-copper nano particle as raw material, it is mixed with surfactant, dispersing agent, solvent and other auxiliary agents,
Conductive ink can be prepared.Using the conductive ink, cost can be significantly reduced, and be able to maintain higher conductivity and anti-oxidant
Property.
Embodiment 2
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, 1- octadecylene is heated to 130 DEG C, keeps the temperature 30min, is then added into the tetradecane of 0.2L
Enter the 1,2- hexadecane two of the copper acetate of 2mmol, the silver acetate of 0.5mmol, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol
Alcohol obtains mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
X-ray diffraction (XRD) figure of silver-copper nano particle obtained by the present embodiment as shown in figure 3, transmission electron microscope (TEM) figure such as
Shown in Fig. 4.
XRD spectrum is shown, containing silver and copper in particle made from the present embodiment, illustrates that the present embodiment is successfully prepared silver-bearing copper
Nano particle, TEM map show that silver-copper nano grain diameter is uniform, but have a little reunion.
Embodiment 3
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, the tetradecane is heated to 130 DEG C, 30min is kept the temperature, is then added into the tetradecane of 0.2L
The copper acetate of 1.5mmol, the silver acetate of 1mmol, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol 1,2- hexadecane diol,
Obtain mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
Embodiment 4
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, the tetradecane is heated to 130 DEG C, 30min is kept the temperature, is then added into the tetradecane of 0.2L
The copper acetate of 2mmol, the silver acetate of 0.5mmol, the oleic acid of 4mmol, the oleyl amine of 4mmol and 4mmol 1,2- hexadecane diol,
Obtain mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
Embodiment 5
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, the tetradecane is heated to 130 DEG C, 30min is kept the temperature, is then added into the tetradecane of 0.2L
The copper acetate of 2mmol, the silver acetate of 0.5mmol, the stearic acid of 2mmol, the oleyl amine of 2mmol and 2mmol 1- octadecanol, obtain
Mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
Embodiment 6
A kind of preparation method of silver-copper nano particle, steps are as follows:
Under the atmosphere of nitrogen, the tetradecane is heated to 100 DEG C, 30min is kept the temperature, is then added into the tetradecane of 0.2L
The copper acetate of 2mmol, the silver acetate of 0.5mmol, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol 1,2- hexadecane diol,
Obtain mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle.
Uniform particle sizes, the silver-copper nano particle of soilless sticking can be successfully prepared in embodiment 3-6.
Comparative example 1
Under the atmosphere of nitrogen, diphenyl ether is heated to 130 DEG C, 30min is kept the temperature, is then added into the diphenyl ether of 0.2L
The copper acetate of 2mmol, the silver acetate of 0.5mmol, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol 1,2- hexadecane diol,
Obtain mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol can not form precipitating.
This comparative example can not prepare silver-copper nano particle using diphenyl ether as solvent.
Comparative example 2
Under the atmosphere of nitrogen, under room temperature, the copper acetate of 2mmol, the acetic acid of 0.5mmol are added into the tetradecane of 0.2L
1, the 2- hexadecane diol of silver, the oleic acid of 2mmol, the oleyl amine of 2mmol and 2mmol, obtains mixture.
Under an inert atmosphere, 200 DEG C are heated the mixture to, 2h is stirred, is cooled to room temperature, reaction is terminated, is then added
Ethyl alcohol forms precipitating, centrifugation, and cleans precipitating for several times with ethane and ethyl alcohol, obtains silver-copper nano particle, still, gained silver-bearing copper is received
Rice grain agglomeration is serious, and partial size is uneven, and yield is few.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of silver-copper nano particle, which comprises the following steps:
Nonpolar solvent is heated to 100 DEG C -150 DEG C, then mantoquita, silver salt, rouge is added in heat preservation into the nonpolar solvent
Fat acid, fatty amine and reducing agent, obtain mixture;
The mixture is heated to 180 DEG C -300 DEG C, cooling after 1h-3h is stirred, alcohols solvent is added, must precipitate, it is as silver-colored
Copper nano particles;
The nonpolar solvent is selected from saturation or unsaturated alkane.
2. preparation method according to claim 1, which is characterized in that the nonpolar solvent is selected from the tetradecane or 1- 18
Alkene.
3. preparation method according to claim 1, which is characterized in that the nonpolar solvent is heated to 100 DEG C -130
℃。
4. preparation method according to claim 1, which is characterized in that the metal salt, fatty acid, fatty amine and reducing agent
The ratio between molal quantity be 5:(4-10): (4-10): (4-10), the molal quantity of the metal salt are mole of the mantoquita and silver salt
The sum of number.
5. the preparation method according to claim 4, which is characterized in that in nonpolar solvent described in 1L, 10mmol- is added
The metal salt of 15mmol.
6. preparation method according to claim 1-5, which is characterized in that the mantoquita is selected from copper acetate;And/
Or,
The silver salt is selected from silver acetate.
7. preparation method according to claim 1-5, which is characterized in that the fatty acid is selected from stearic acid, palm fibre
One or more of palmitic acid acid, myristic acid, lauric acid and oleic acid;And/or
The fatty amine is oleyl amine.
8. preparation method according to claim 1-5, which is characterized in that the reducing agent is selected from 1- octadecane
One or more of alcohol, oleyl alcohol and 1,2- hexadecane diol;And/or
The alcohols solvent is ethyl alcohol.
9. a kind of nano silver copper particle, which is characterized in that be made by the described in any item preparation methods of claim 1-8.
10. a kind of ink, which is characterized in that its raw material includes nano silver copper particle as claimed in claim 9.
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Cited By (3)
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CN110681872A (en) * | 2019-09-27 | 2020-01-14 | 昆明理工大学 | Preparation method of copper/silver corn-shaped structure nanoparticles |
CN111659900A (en) * | 2020-05-09 | 2020-09-15 | 苏州英纳电子材料有限公司 | Nano silver particle and preparation method thereof |
CN111748243A (en) * | 2020-08-15 | 2020-10-09 | 明鑫(深圳)技术研究有限公司 | Conductive ink, preparation method thereof and flexible heater |
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CN111748243A (en) * | 2020-08-15 | 2020-10-09 | 明鑫(深圳)技术研究有限公司 | Conductive ink, preparation method thereof and flexible heater |
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