CN105462365A - Electric conduction nanometer copper ink preparation method - Google Patents
Electric conduction nanometer copper ink preparation method Download PDFInfo
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- CN105462365A CN105462365A CN201410460469.3A CN201410460469A CN105462365A CN 105462365 A CN105462365 A CN 105462365A CN 201410460469 A CN201410460469 A CN 201410460469A CN 105462365 A CN105462365 A CN 105462365A
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Abstract
The present invention discloses an electric conduction nanometer copper ink preparation method, which comprises: (1) sequentially adding polyvinylpyrrolidone, freshly-prepared copper hydroxide and glycerol to a first solvent to form a mixed solution; (2) adding the mixed solution obtained in the step (1) into a an autoclave, and carrying out a reaction for 2-24 h at a temperature of 80-250 DEG C to obtain a nanometer copper dispersion liquid; (3) carrying out a centrifugation treatment on the nanometer copper dispersion liquid, washing the obtained precipitate by using a second solvent, and carrying out vacuum drying to obtain copper nanoparticles; and (4) dispersing the obtained copper nanoparticles in a third solvent to form the electric conduction nanometer copper ink. According to the present invention, the inexpensive glycerol is adopted as the reducing agent to prepare the electric conduction nanometer copper ink, such that the method has characteristics of simple process, easy operation, safety, no toxicity, green environmental protection, low cost, controlled reaction process, no impurity introducing during the reaction, high yield, and simple and mild reaction conditions, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of conductive ink, particularly relate to a kind of preparation method of conducting nano copper ink, belong to technical field of nano material.
Technical background
Metal nano material is field the most popular in current Materials science research.This is because, compared with body material, the metallics (as Au, Ag, Cu etc.) of nano-scale has that size is little, specific surface area is large, resistance is little and the feature such as quantum size effect, macro quanta tunnel effect, makes it show good application prospect in fields such as optics, mechanics, medical science, electricity, mechanochemistries.As the functional materials of a class outbalance, Nanometer Copper is used widely because of advantages such as its superior performance, toxicity are little, cheap in industrial production, daily life, more becomes the focus of preparation and research.
Carried out a lot of work to the research of Nanometer Copper both at home and abroad, the preparation of Nanometer Copper always is the focus of research.At present, the most frequently used synthetic method is polyol process, the precipitator method, hydrothermal method, sonochemistry method, microemulsion method and chemical reduction method etc.In these methods, usually need to add reductive agent as formaldehyde, hydrazine hydrate, inferior sodium phosphate, sodium borohydride, xitix, glucose etc., and in these conventional reductive agents, some are highly toxic substance (as: hydrazine hydrate, formaldehyde etc.), some easily introduce other impurity (as: inferior sodium phosphate, sodium borohydride etc.) when reacting, and some costs are high or easily decompose (as: xitix, glucose etc.) at relatively high temperatures.These become one of important factor of restriction Nanometer Copper suitability for industrialized production.
Publication No. is the preparation method that the patent of invention of CN103341633A reports a kind of conductive ink nanometer copper, copper source and polyoxyethylene glycol are added reductive agent L-AA by the method under the condition of heated and stirred, and then continue heated and stirred and obtain copper nano particles, although reaction conditions is gentle, but the temperature range of reaction is narrower, need to stir and just can obtain finely dispersed copper nano particles, but the reductive agent L-AA cost adopted is high, causes the with high costs of suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of conducting nano copper ink, this preparation method be simple to operation, cost is low, environmentally friendly, and obtain conductive copper ink there is good oxidation-resistance and dispersiveness, be applicable to large-scale industrial production.
For realizing aforementioned invention object, the technical solution used in the present invention comprises:
A preparation method for conducting nano copper ink, comprises the steps:
(1) copper hydroxide of polyvinylpyrrolidone, fresh preparation and glycerol are joined in the first solvent successively, form mixing solutions;
(2) step (1) mixing solutions that obtains being added autoclave, such as, in tetrafluoroethylene autoclave tank, is react 2h ~ 24h under the condition of 80 ~ 250 DEG C in temperature, obtains Nanometer Copper dispersion liquid;
(3) centrifugal treating is carried out to described Nanometer Copper dispersion liquid, and with the second throw out that solvent wash obtains, after vacuum-drying, obtain nanometer copper particle;
(4) described nanometer copper particle is scattered in the 3rd solvent, forms described conducting nano copper ink.
As one of comparatively preferred embodiment, be the copper hydroxide of the fresh preparation of 0.05-0.2M containing concentration in mixing solutions described in step (1).
As one of comparatively preferred embodiment, in step (1), the copper hydroxide of fresh preparation and the mass ratio of polyvinylpyrrolidone are 0.05-0.2.
As one of comparatively preferred embodiment, containing concentration in mixing solutions described in step (1) is the glycerol of 0.3M ~ 6.6M.
Further, described polyvinylpyrrolidone can be selected from but be not limited to K-15, any one or two or more combinations in K-30, K-60, K-90.
Further, described first solvent can be selected from but be not limited to any one or the two or more combinations in water, ethanol, ethylene glycol and glycol ether.
As one of comparatively preferred embodiment, step (3) comprising: with the rotating speed of 8000 ~ 15000 revs/min to after described Nanometer Copper dispersion liquid centrifugal treating 20 ~ 30min, then obtain throw out with the second solvent wash.
Further, described second solvent can be selected from but be not limited to any one or the two or more combinations in water, dehydrated alcohol and acetone.
Further, described 3rd solvent can be selected from but be not limited to any one or the two or more combinations in dehydrated alcohol, methyl alcohol, acetone, ethyl acetate, Virahol, normal hexane, heptane, propylene glycol, ethylene glycol, glycol ether, cellosolvo.
As one of comparatively preferred embodiment, the preparation method of described conducting nano copper ink comprises:
A, mantoquita to be dissolved in the water, under accompanying by the condition of stirring, slowly to add ammoniacal liquor at normal temperature, until the light blue precipitation produced is dissolved completely, then add strong base solution, generate blue copper hydroxide precipitation,
Described copper hydroxide precipitation is isolated in b, employing, after washing, obtains the copper hydroxide of described fresh preparation.
Further, described mantoquita can be selected from but be not limited to any one or the two or more combinations in copper sulfate, cupric chloride, neutralized verdigris, cupric nitrate.
Further, described mantoquita strong base solution can be selected from but be not limited to sodium hydroxide or potassium hydroxide solution.
Further, the cleaning solvent adopted in step b can be selected from but be not limited to water and/or dehydrated alcohol.
Such as, in a case study on implementation, refer to Fig. 1, the preparation method of described conducting nano copper ink can comprise the following steps:
Step 1: be dissolved in by compound nantokite in distilled water, under stirring at normal temperature condition, drips ammonia soln, until the light blue precipitation produced is dissolved completely;
Step 2: aqueous sodium hydroxide solution is added step 1 obtain in solution, generate blue copper hydroxide precipitation, suction filtration, washing, obtains the copper hydroxide of fresh preparation;
Step 3: by polyvinylpyrrolidone, step 2 obtain the copper hydroxide of fresh preparation and reductive agent glycerol joins in the first solvent (showing in figure for A) successively;
Step 4: mixing solutions step 3 obtained joins in tetrafluoroethylene autoclave tank, under 80 ~ 250 DEG C of conditions, reaction 2h ~ 24h, obtains Nanometer Copper dispersion liquid;
Step 5: after step 4 being obtained Nanometer Copper dispersion liquid centrifugal treating, with the second solvent (also can be described as solvent B) washing, is placed in vacuum drying oven dry, obtains Nanometer Copper.
Step 6: Nanometer Copper step 5 obtained is scattered in the 3rd solvent (also can be described as solvent C), obtains described conducting nano copper ink.
Compared with prior art, advantage of the present invention comprises:
(1) preparation method of this conducting nano copper ink adopts glycerol as reductive agent, nontoxic, and cost is low, can not introduce other impurity in the reaction, productive rate is high, and reaction conditions is simply gentle, the conductive ink of preparation has resistance of oxidation, is applicable to large-scale industrial production.
(2) reaction unit that the preparation method of this conducting nano copper ink adopts is autoclave, the conducting nano copper ink that class is spherical, single dispersing degree is high can be obtained under without the condition stirred, temperature range widely can be utilized simultaneously, the particle diameter of Nanometer Copper and the carrying out of pattern are controlled;
(3) preparation method of this conducting nano copper ink adopts the copper hydroxide of fresh preparation as one of reaction raw materials, compared with commercially available copper hydroxide, particle is small, and surface-area is large, reactive behavior is high, makes the even size distribution of the nanometer copper particle of acquisition and purity is high.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is preparation technology's schema of a kind of conducting nano copper ink in the present invention one typical embodiments;
Fig. 2 be embodiment 1 obtain the XRD figure of nanometer copper particle;
Fig. 3 be embodiment 1 obtain nanometer copper particle SEM figure;
Fig. 4 be embodiment 1 obtain the particle size distribution figure of nanometer copper particle.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be described in detail the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
embodiment 1
(1) be dissolved in the distilled water of 100ml by the copper sulfate of 0.05mol, drip the ammoniacal liquor that 30ml volume ratio is 1:1 under stirring at normal temperature condition, until the blue precipitate produced just dissolves completely, solution becomes mazarine;
(2) slowly join in above-mentioned solution by the sodium hydroxide solution of 50ml0.1mol, generate blue copper hydroxide precipitation, deionized water and dehydrated alcohol wash 3 times respectively, can obtain the copper hydroxide of fresh preparation;
(3) PVP K-30 of 1.9g, the freshly prepd copper hydroxide of 0.3g and 5M ~ 6.6M reductive agent glycerol are joined in the dehydrated alcohol of 30ml successively;
(4) joined by the solution mixed in tetrafluoroethylene autoclave tank, under 80 ~ 100 DEG C of conditions, reaction 20 ~ 24h, can obtain Nanometer Copper dispersion liquid;
(5) by Nanometer Copper dispersion liquid under the rotating speed of 8000 ~ 10000 revs/min, after centrifugal 20 ~ 30 minutes, with absolute ethanol washing 3 times, be placed in vacuum drying oven in temperature 30 ~ 50 DEG C, dry 2 ~ 3h, target product nanometer copper particle (following be called for short " Nanometer Copper ");
(6) Nanometer Copper is scattered in solvent dehydrated alcohol, obtains conductive nano copper ink.
embodiment 2
(1) be dissolved in the distilled water of 100ml by the cupric chloride of 0.05mol, drip the ammoniacal liquor that 30ml volume ratio is 1:1 under stirring at normal temperature condition, until the blue precipitate produced just dissolves completely, solution becomes mazarine.
(2) slowly join in above-mentioned solution by the sodium hydroxide solution of 50ml0.1mol, generate blue copper hydroxide precipitation, deionized water and dehydrated alcohol wash 3 times respectively, can obtain the copper hydroxide of fresh preparation;
(3) the freshly prepd copper hydroxide of polyvinylpyrrolidone K-15,0.6g of 12g and 3.3M ~ 5M reductive agent glycerol are joined in the deionized water of 30ml successively;
(4) joined by the solution mixed in tetrafluoroethylene autoclave tank, under 100 ~ 150 DEG C of conditions, reaction 12 ~ 20h, can obtain Nanometer Copper dispersion liquid;
(5) by Nanometer Copper dispersion liquid under the rotating speed of 10000 ~ 12000 revs/min, with deionized water wash 3 times after centrifugal 10 ~ 20 minutes, be placed in vacuum drying oven in temperature 50 ~ 70 DEG C, dry 1 ~ 2h, can obtain target product Nanometer Copper.
(6) Nanometer Copper is scattered in solvent ethylene glycol, obtains conducting nano copper ink.
embodiment 3
(1) be dissolved in the distilled water of 100ml by the cupric nitrate of 0.05mol, drip the ammoniacal liquor that 30ml volume ratio is 1:1 under stirring at normal temperature condition, until the blue precipitate produced just dissolves completely, solution becomes mazarine.
(2) slowly join in above-mentioned solution by the sodium hydroxide solution of 50ml0.1mol, generate blue copper hydroxide precipitation, deionized water and dehydrated alcohol wash 3 times respectively, can obtain the copper hydroxide of fresh preparation;
(3) the freshly prepd copper hydroxide of polyvinylpyrrolidone K-60,0.44g of 2.2g and 1.7M ~ 3.3M reductive agent glycerol are joined in the ethylene glycol of 30ml successively;
(4) joined by the solution mixed in tetrafluoroethylene autoclave tank, under 150 ~ 200 DEG C of conditions, reaction 6 ~ 12h, can obtain Nanometer Copper dispersion liquid;
(5) by Nanometer Copper dispersion liquid under the rotating speed of 12000 ~ 15000 revs/min, after centrifugal 5 ~ 10 minutes, with washing with acetone 3 times, be placed in vacuum drying oven in temperature 70 ~ 80 DEG C, dry 0.5 ~ 1h, can obtain product nano copper.
(6) Nanometer Copper is scattered in solvent glycol ether, obtains conducting nano copper ink.
embodiment 4
(1) be dissolved in the distilled water of 100ml by the neutralized verdigris of 0.05mol, drip the ammoniacal liquor that 30ml volume ratio is 1:1 under stirring at normal temperature condition, until the blue precipitate produced just dissolves completely, solution becomes mazarine.
(2) slowly join in above-mentioned solution by the sodium hydroxide solution of 50ml0.1mol, generate blue copper hydroxide precipitation, deionized water and dehydrated alcohol wash 3 times respectively, can obtain the copper hydroxide of fresh preparation;
(3) PVP K-90 of 0.3g, the freshly prepd copper hydroxide of 0.03g and 0.3M ~ 1.7M reductive agent glycerol are joined in the glycol ether of 30ml successively;
(4) joined by the solution mixed in tetrafluoroethylene autoclave tank, under 200 ~ 250 DEG C of conditions, reaction 3 ~ 6h, can obtain Nanometer Copper dispersion liquid;
(5) by Nanometer Copper dispersion liquid under the rotating speed of 8000 ~ 10000 revs/min, after centrifugal 20 ~ 30 minutes, with absolute ethanol washing 3 times, be placed in vacuum drying oven in temperature 30 ~ 50 DEG C, dry 2 ~ 3h, can obtain target product Nanometer Copper.
(6) Nanometer Copper is scattered in solvent glycol ether, obtains conducting nano copper ink.
It should be noted that, in this article, the such as relational terms of first and second grades and so on is only used for an entity or operation to separate with another entity or operational zone, and not necessarily requires or imply the relation that there is any this reality between these entities or operation or sequentially.And, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within process, method, article or the equipment comprising described key element and also there is other identical element.
The above is only the specific embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (12)
1. a preparation method for conducting nano copper ink, is characterized in that comprising the steps:
(1) copper hydroxide of polyvinylpyrrolidone, fresh preparation and glycerol are joined in the first solvent successively, form mixing solutions;
(2) adding in autoclave by step (1) mixing solutions that obtains, is react 2h ~ 24h under the condition of 80 ~ 250 DEG C in temperature, obtains Nanometer Copper dispersion liquid;
(3) centrifugal treating is carried out to described Nanometer Copper dispersion liquid, and with the second throw out that solvent wash obtains, after vacuum-drying, obtain nanometer copper particle;
(4) described nanometer copper particle is scattered in the 3rd solvent, forms described conducting nano copper ink.
2. the preparation method of conducting nano copper ink according to claim 1, it is characterized in that, be the copper hydroxide of the fresh preparation of 0.05-0.2M containing concentration in mixing solutions described in step (1), and the mass ratio of the copper hydroxide of fresh preparation and polyvinylpyrrolidone is 0.05-0.2.
3. the preparation method of conducting nano copper ink according to claim 1, is characterized in that containing concentration in mixing solutions described in step (1) is the glycerol of 0.3M ~ 6.6M.
4. the preparation method of the conducting nano copper ink according to any one of claim 1-3, is characterized in that described polyvinylpyrrolidone comprises K-15, any one or two or more combinations in K-30, K-60, K-90.
5. the preparation method of the conducting nano copper ink according to any one of claim 1-3, is characterized in that described first solvent comprises any one or two or more combinations in water, ethanol, ethylene glycol and glycol ether.
6. the preparation method of conducting nano copper ink according to claim 1, it is characterized in that step (3) comprising: with the rotating speed of 8000 ~ 15000 revs/min to after described Nanometer Copper dispersion liquid centrifugal treating 20 ~ 30min, then obtain throw out with the second solvent wash.
7. the preparation method of the conducting nano copper ink according to claim 1 or 6, is characterized in that described second solvent comprises any one or two or more combinations in water, dehydrated alcohol and acetone.
8. the preparation method of conducting nano copper ink according to claim 1, is characterized in that the vacuum-drying temperature adopted in step (3) is 30 ~ 80 DEG C.
9. the preparation method of conducting nano copper ink according to claim 1, is characterized in that described 3rd solvent comprises any one or two or more combinations in dehydrated alcohol, methyl alcohol, acetone, ethyl acetate, Virahol, normal hexane, heptane, propylene glycol, ethylene glycol, glycol ether, cellosolvo.
10. the preparation method of conducting nano copper ink according to claim 1, is characterized in that comprising:
A, mantoquita to be dissolved in the water, under accompanying by the condition of stirring, slowly to add ammoniacal liquor at normal temperature, until the light blue precipitation produced is dissolved completely, then add strong base solution, generate blue copper hydroxide precipitation,
B, isolate described copper hydroxide precipitation, through washing after, obtain the copper hydroxide of described fresh preparation.
The preparation method of 11. conducting nano copper inks according to claim 10, is characterized in that described mantoquita comprises any one or two or more combinations in copper sulfate, cupric chloride, neutralized verdigris, cupric nitrate.
The preparation method of 12. conducting nano copper inks according to claim 10, is characterized in that the cleaning solvent adopted in step b comprises water and/or dehydrated alcohol.
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| CN106205772A (en) * | 2016-07-01 | 2016-12-07 | 中国科学院深圳先进技术研究院 | Cuprio electrocondution slurry and preparation and its application in chip package copper copper is bonded |
| CN106280716A (en) * | 2016-10-31 | 2017-01-04 | 南京东纳生物科技有限公司 | The preparation method and applications of the conductive silver ink that a kind of surface enhanced raman spectroscopy is sensitive |
| CN107445149A (en) * | 2016-05-31 | 2017-12-08 | 嘉泉大学校产学协力团 | Graphene metal nanoparticle complex |
| CN109651892A (en) * | 2019-01-28 | 2019-04-19 | 哈尔滨工业大学（威海） | A kind of preparation method of nano-copper conductive ink |
| CN109940169A (en) * | 2019-04-19 | 2019-06-28 | 陕西科技大学 | A kind of Nanometer Copper and preparation method thereof |
| CN111906329A (en) * | 2020-09-01 | 2020-11-10 | 中国科学院深圳先进技术研究院 | Preparation method of copper nano material structure |
| CN112276107A (en) * | 2019-07-25 | 2021-01-29 | 上海沪正实业有限公司 | Nano-copper particles and application thereof in preparation of nano-copper fabric after-finishing agent |
| CN113545778A (en) * | 2021-07-05 | 2021-10-26 | 张智祺 | Porous blood sugar electrode material and preparation method thereof |
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| CN112276107A (en) * | 2019-07-25 | 2021-01-29 | 上海沪正实业有限公司 | Nano-copper particles and application thereof in preparation of nano-copper fabric after-finishing agent |
| CN111906329A (en) * | 2020-09-01 | 2020-11-10 | 中国科学院深圳先进技术研究院 | Preparation method of copper nano material structure |
| CN113545778A (en) * | 2021-07-05 | 2021-10-26 | 张智祺 | Porous blood sugar electrode material and preparation method thereof |
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Application publication date: 20160406 |