CN103341633A - Method for preparing conductive ink nanometer copper - Google Patents
Method for preparing conductive ink nanometer copper Download PDFInfo
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- CN103341633A CN103341633A CN2013102528436A CN201310252843A CN103341633A CN 103341633 A CN103341633 A CN 103341633A CN 2013102528436 A CN2013102528436 A CN 2013102528436A CN 201310252843 A CN201310252843 A CN 201310252843A CN 103341633 A CN103341633 A CN 103341633A
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Abstract
The invention discloses a method for preparing conductive ink nanometer copper. The method includes the steps that a copper source is added to a solvent A at the concentration of 0.05-0.5 mol/L, 5-20ml polyethylene glycol is added, the mixture is evenly stirred and then heated to 60-160 DEG C, and a solution a is obtained; L-ascorbic acid is added to a solvent B at the concentration of 0.5-1.0mol/L, the mixture is evenly stirred and then heated to 60-160 DEG C, and a solution b is obtained; the solution B is added to the solution a, the mixture is continued to be stirred for 5min-5h and then cooled to indoor temperature, vacuum drying is performed after centrifugation, and the conductive ink nanometer copper is obtained. Ethyl alcohol or polyhydric alcohol serves as the solvent, the L-ascorbic acid which is cheap and easy to get serves as a reducing agent and a protective agent, and nanometer copper particles are prepared. Reaction conditions are simple and mild, the particle size and the morphology of the nanometer copper are easy to control, generation, agglomeration preventing and oxidation resistance of the nanometer copper are achieved synchronously, and the prepared conductive ink nanometer copper is good in dispersibility and high in single dispersity, and has oxidation resistance to a certain extent. The method can be applied to large-scale production.
Description
[technical field]
The invention belongs to the technical field of nano metal material, particularly a kind of preparation method of electrically conductive ink nanometer copper.
[background technology]
Nano metal printing ink has that particle diameter is little, sintering temperature is low (generally only being 100~300 ℃), sinter line into after conductance than characteristics such as height, be the primary raw material of printed electronics technology of new generation.At present, document has been reported the multiple metallic conduction printing ink that comprises nm of gold, Nano Silver, nanometer copper.Nanometer copper is because it is cheap, and characteristics such as difficult generation ion migration have attracted numerous researchers' interest.
The common method for preparing nanometer copper has sol-gel process, hydrothermal reduction method, electrolysis, plasma method, gas phase steam method, thermal decomposition method and liquid phase reduction etc.The sol-gel process reaction temperature is low, and the product particle is little, narrow particle size distribution and purity height, but cost is higher and follow pollution; The particle purity height that the hydrothermal reduction method obtains, narrow particle size distribution, and lattice growth is complete pollution-free, but higher to proportion of raw materials and purity requirement, be not suitable for large-scale production; The preparation technology of electrolysis is simple relatively, but last handling process is comparatively loaded down with trivial details; The reaction temperature height of plasma method, reaction speed is fast, and is simple to operate and speed of production is fast, but energy consumption is bigger; With respect to additive method, thermal decomposition method is faster, economical and green, but wayward copper particle grain size and pattern.Chemical reduction method can be by optimizing the nano copper particle that technology obtains different-grain diameter and pattern, used reducing agent is generally sodium borohydride, formaldehyde, hydrazine hydrate or sodium hypophosphite etc., these reducing agents are expensive, and all have bigger toxicity mostly, are unfavorable for large-scale production.
Patent 200510094614.1 discloses a kind of method for preparing nanometer copper, this method is soluble in water with reducing agent L-ascorbic acid and composite dressing agent, be added dropwise to copper source solution after adding hot reflux a few hours, continue back flow reaction again and obtain nanometer copper, its reaction condition gentleness, but need to reflux repeatedly heating, complicated operation is loaded down with trivial details.Patent application 200910054884.8 discloses a kind of preparing nano copper conductive, and this method is carried out post processing by electrodialysis and decompression distillation, the operating procedure complexity, and manufacturing cycle is long.Patent 201010221315.0 discloses a kind of preparing nano copper conductive, though this method need not loaded down with trivial details post processing, complicated process of preparation.
At present, do not have still that a kind of preparation technology is simple, cost is low and can be applied to the report about the preparation method of electrically conductive ink nanometer copper of large-scale production.
[summary of the invention]
The objective of the invention is to overcome the shortcoming and defect that prior art exists, a kind of preparation method of electrically conductive ink nanometer copper is provided.The preparation technology of this method is simple, with low cost, environmental friendliness and can be applied to large-scale production.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of electrically conductive ink nanometer copper, comprise the steps: the copper source is added in the solvent orange 2 A by 0.05~0.5mol/L, add 5~20ml polyethylene glycol (PEG), be heated to 60~160 ℃ after stirring, obtain solution a; The L-ascorbic acid is added among the solvent B by 0.5~1.0mol/L, be heated to 60~160 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5min~5h, centrifugal, get precipitation, spend deionised water final vacuum drying, obtain electrically conductive ink nanometer copper; The mol ratio of copper source and L-ascorbic acid is 1:1~1:20.
Described copper source is preferably at least a in Kocide SD, copper nitrate, acetylacetone copper, copper sulphate or the copper chloride.
Described solvent orange 2 A is preferably a kind of or at least two kinds of mixtures in ethanol, ethylene glycol, diglycol, Diethylene Glycol, dipropylene glycol and the glycerine.
Described polyethylene glycol is preferably a kind of or at least two kinds of mixtures among PEG-200, PEG-400, PEG-600 and the PEG-800.Polyethylene glycol mainly is to use as protective agent and dispersant.
Described solvent B is preferably a kind of or at least two kinds of mixtures in ethanol, ethylene glycol, diglycol, Diethylene Glycol, dipropylene glycol and the glycerine.
The solvent of described washing is preferably a kind of or at least two kinds of mixtures in deionized water, absolute ethyl alcohol or the acetone.
Preferably, described solvent orange 2 A and solvent B are with a kind of solvent.
Preferably, described solution a is identical with the temperature of solution b.
Described centrifugal condition is preferably the centrifuge washing in 3000~8000r/min;
The number of times of described centrifuge washing is preferably 4 times.
Described vacuum drying condition is preferably in vacuum less than 0.01MPa, drying at room temperature 6h~12h.
The present invention has following advantage and beneficial effect with respect to prior art:
(1) the present invention is that solvent, L-ascorbic acid cheap and easy to get prepare nano copper particle as reducing agent and protective agent with ethanol or polyalcohol; reaction condition is simply gentle; particle diameter and the pattern of nanometer copper are controlled easily; and the generation of nanometer copper, prevent from reuniting and anti-oxidant synchronous realization; the electrically conductive ink nanometer copper good dispersion for preparing; single decentralization height, and have to a certain degree oxidation resistance, can be applicable to large-scale production.
(2) raw material of the present invention be easy to get, easy and simple to handle, cost is low, environmental friendliness, uses the electrically conductive ink nanometer shot copper footpath of the inventive method preparation little, conductance is high, can be applicable to fields such as electrically conductive ink and printed electronics technology.
[description of drawings]
Fig. 1 is X-ray diffraction (XRD) spectrogram of the nanometer copper of embodiment 1 preparation.
Fig. 2 is field emission scanning electron microscope (SEM) figure of the nanometer copper of embodiment 1 preparation; Wherein: a is the field emission scanning electron microscope figure (* 10000) of nanometer copper, and b is the field emission scanning electron microscope figure (* 20000) of nanometer copper.
Fig. 3 is field emission scanning electron microscope (SEM) figure of the nanometer copper of embodiment 5 preparations; Wherein: a is the field emission scanning electron microscope figure (* 10000) of nanometer copper, and b is the field emission scanning electron microscope figure (* 20000) of nanometer copper.
Fig. 4 is field emission scanning electron microscope (SEM) figure of the nanometer copper of embodiment 8 preparations; Wherein: a is the field emission scanning electron microscope figure (* 10000) of nanometer copper, and b is the field emission scanning electron microscope figure (* 20000) of nanometer copper.
[specific embodiment]
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Embodiment 1
Kocide SD 0.20g is added in the 40ml ethanol, add 20ml PEG-200, be heated to 60 ℃ after stirring, obtain solution a; 3.52g L-ascorbic acid is added in the 40ml ethanol, be heated to 60 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5min, 3000r/min deionized water centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 6h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Get the above-mentioned nanometer copper that obtains, use x-ray diffractometer (XRD) that particle is carried out thing phase atlas analysis, use field emission scanning electron microscope (SEM) to observe the pattern of particle, the result as depicted in figs. 1 and 2.The characteristic peak of copper as can see from Figure 1 is wherein without any the characteristic peak of cuprous oxide or cupric oxide grade in an imperial examination two-phase impurity; As can be seen from Figure 2 the particle diameter of this nanometer copper is at 100~200nm, and the particle good dispersion does not have tangible agglomeration.
Copper sulphate 0.64g is added in the 40ml ethylene glycol, add 15ml PEG-400, be heated to 80 ℃ after stirring, obtain solution a; 4.23g L-ascorbic acid is added in the 40ml ethylene glycol, be heated to 80 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 30min, 5000r/min absolute ethyl alcohol centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 6h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 3
Acetylacetone copper 2.09g is added in the 40ml diglycol, add 10ml PEG-600, be heated to 100 ℃ after stirring, obtain solution a; 4.93g L-ascorbic acid is added in the 40ml diglycol, be heated to 100 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 1h, 8000r/min acetone centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 6h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Copper nitrate 2.90g is added in the 40ml Diethylene Glycol, add 5ml PEG-800, be heated to 120 ℃ after stirring, obtain solution a; 5.64g L-ascorbic acid is added in the 40ml Diethylene Glycol, be heated to 120 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 3h, 3000r/min absolute ethyl alcohol centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 8h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 5
Kocide SD 1.95g is added in the 40ml glycerine, add 15ml PEG-600, be heated to 60 ℃ after stirring, obtain solution a; 7.05g L-ascorbic acid is added in the 40ml glycerine, be heated to 60 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5h, 5000r/min deionized water centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 8h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 6
Copper chloride 2.73g is added in the 40ml dipropylene glycol, add 20ml PEG-800, be heated to 160 ℃ after stirring, obtain solution a; 6.23g L-ascorbic acid is added in the 40ml dipropylene glycol, be heated to 160 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5h, 8000r/min absolute ethyl alcohol centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 8h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 7
Copper sulphate 0.32g is added in the 40ml ethylene glycol, add 10ml PEG-400, be heated to 80 ℃ after stirring, obtain solution a; 7.05g L-ascorbic acid is added in the 40ml ethylene glycol, be heated to 80 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 3h, 3000r/min acetone centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 12h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and SEM figure and the embodiment 1 shows that the thing of this nanometer copper is fine copper mutually, do not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 8
Acetylacetone copper 1.57g is added in the 40ml diglycol, add 5ml PEG-200, be heated to 100 ℃ after stirring, obtain solution a; 5.64g L-ascorbic acid is added in the 40ml diglycol, be heated to 100 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 1h, 5000r/min deionized water centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 12h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and the embodiment 1, SEM schemes as shown in Figure 4.The thing that shows this nanometer copper is fine copper mutually, does not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Embodiment 9
Copper nitrate 2.42g is added in the 40ml Diethylene Glycol, add 20ml PEG-400, be heated to 120 ℃ after stirring, obtain solution a; 4.23g L-ascorbic acid is added in the 40ml Diethylene Glycol, be heated to 120 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 30min, 8000r/min absolute ethyl alcohol centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 12h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and the embodiment 1, SEM scheme and embodiment 8 in similar.The thing that shows this nanometer copper is fine copper mutually, does not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
Copper chloride 3.41g is added in the 40ml dipropylene glycol, add 20ml PEG-600, be heated to 160 ℃ after stirring, obtain solution a; 3.52g L-ascorbic acid is added in the 40ml dipropylene glycol, be heated to 160 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5min, 8000r/min acetone centrifuge washing 4 times is got and is deposited in vacuum less than drying at room temperature 6h under the condition of 0.01MPa, obtains electrically conductive ink nanometer copper;
Similar among the XRD of the nanometer copper for preparing figure and the embodiment 1, SEM scheme and embodiment 8 in similar.The thing that shows this nanometer copper is fine copper mutually, does not have other second phase impurity; The particle good dispersion does not have tangible agglomeration.
The above the specific embodiment of the present invention does not constitute the restriction to protection domain of the present invention.Various other corresponding changes and distortion that any technical conceive according to the present invention has been done all should be included in the protection domain of claim of the present invention.
Claims (8)
1. the preparation method of an electrically conductive ink nanometer copper is characterized in that comprising the steps: the copper source is added in the solvent orange 2 A by 0.05~0.5mol/L, adds 5~20ml polyethylene glycol, is heated to 60~160 ℃ after stirring, and obtains solution a; The L-ascorbic acid is added among the solvent B by 0.5~1.0mol/L, be heated to 60~160 ℃ after stirring, obtain solution b; Solution b is added among the solution a, be cooled to room temperature after continuing to stir 5min~5h, centrifugal, get precipitation, washing final vacuum drying obtains electrically conductive ink nanometer copper; The mol ratio of copper source and L-ascorbic acid is 1:1~1:20.
2. the preparation method of electrically conductive ink nanometer copper according to claim 1 is characterized in that: described copper source is at least a in Kocide SD, copper nitrate, acetylacetone copper, copper sulphate or the copper chloride.
3. the preparation method of electrically conductive ink nanometer copper according to claim 1, it is characterized in that: described solvent orange 2 A is a kind of or at least two kinds of mixtures in ethanol, ethylene glycol, diglycol, Diethylene Glycol, dipropylene glycol and the glycerine.
4. the preparation method of electrically conductive ink nanometer copper according to claim 1, it is characterized in that: described polyethylene glycol is a kind of or at least two kinds of mixtures among PEG-200, PEG-400, PEG-600 and the PEG-800.
5. the preparation method of electrically conductive ink nanometer copper according to claim 1, it is characterized in that: described solvent B is a kind of or at least two kinds of mixtures in ethanol, ethylene glycol, diglycol, Diethylene Glycol, dipropylene glycol and the glycerine.
6. the preparation method of electrically conductive ink nanometer copper according to claim 1 is characterized in that: described centrifugal condition is in 3000~8000r/min centrifuge washing.
7. according to the preparation method of claim 1 or 6 described electrically conductive ink nanometer copper, it is characterized in that: the solvent of described washing is a kind of or at least two kinds of mixtures in deionized water, absolute ethyl alcohol or the acetone.
8. the preparation method of electrically conductive ink nanometer copper according to claim 1 is characterized in that: described vacuum drying condition in vacuum less than 0.01MPa, drying at room temperature 6~12h.
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