CN106700735A - Non-particle conductive copper ink capable of being heated in air and preparation and use method thereof - Google Patents
Non-particle conductive copper ink capable of being heated in air and preparation and use method thereof Download PDFInfo
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- CN106700735A CN106700735A CN201611096605.0A CN201611096605A CN106700735A CN 106700735 A CN106700735 A CN 106700735A CN 201611096605 A CN201611096605 A CN 201611096605A CN 106700735 A CN106700735 A CN 106700735A
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Abstract
The invention relates to a non-particle conductive copper ink capable of being heated in air and a preparation and use method thereof, and belongs to the technical field of conductive ink. The non-particle conductive copper ink is prepared from the following components in percentage by mass: 20 to 73% of copper precursor, 15 to 60% of complexing agent, 10 to 51% of solvent, and 0 to 10% of additive. The preparation method comprises the following steps of adding the complexing agent into the additive and the solvent, uniformly mixing, adding the copper precursor, stirring, and filtering by a microporous filter membrane, so as to obtain the non-particle conductive copper ink. The use method comprises the following steps of printing or coating the conductive copper ink onto a substrate, performing heat treatment for 1 to 15min at the temperature of 130 to 350 DEG C, and sintering, so as to obtain a copper thin film/copper conducting wire which is stuck on the substrate. The non-particle conductive copper ink has the advantages that any solid particle is not contained, the stability is high, the conductivity is good, the preparation method is simple, and the operation is easy. The preparation method has the advantages that the non-particle conductive copper ink can be heated in air to obtain pure copper, the curing temperature is low, the time is short, the pollution is avoided, the cost is low, and the preparation method is suitable for realizing industrialization.
Description
Technical field
The invention belongs to conductive ink technology field, more particularly to it is a kind of can heat in atmosphere without particle conductive copper ink
Water and its preparation and application.
Background technology
Printed electronics (printed electronics) refer to use printing means, by conducting polymer, nano metal ink
The functional material ink such as water or nano-inorganic substance is printed on base material, is a kind of low cost, is expeditiously manufactured circuit and electricity
The technology of sub- device.
In numerous conductive inks, conducting polymer has a low advantage of sintering temperature, but its conductance is low and chemistry
Stability is low and then limits its development.In in recent years, carbon material ink is received significant attention, mainly due to its low cost,
But its relatively low conductance can not be satisfied with the device for needing high conductivity.For apply wider metallic based inks, gold,
Silver, copper ink obtain extensive concern.Gold and silver inks water enjoy favor because it has inoxidizability higher.However, in order to drop
Low cost, researchers also replace Jin Heyin from the relatively low copper of resistivity, yet with copper property oxidizable in atmosphere
Copper-based ink is sintered densification by matter, people's majority under inert gas, reducibility gas or vacuum environment, and this is virtually multiple
Miscellaneous operating procedure, and reducibility gas are relatively hazardous.And copper-based conductive ink involved in the present invention be by copper-based presoma,
Solvent and some auxiliary agents are constituted, and are blue liquid, do not contain any particulate matter, and stability is high, can be by various printing electricity
The means or technology for coating of son are printed to line or pattern on substrate, and obtain conductive copper in atmosphere by subsequent heat treatment
Line, is with a wide range of applications in terms of printed electronics.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide it is a kind of can heat in atmosphere without particle conductive copper ink and its
Preparation and application, the ink does not contain any solid particle, and stability is high, and good conductivity, preparation method is simple to operation.
The preparation method can in atmosphere be heated and obtain elemental copper, and solidification temperature is low, and the time is short, pollution-free, with low cost, it is easy to accomplish
Industrialization.
It is of the invention it is a kind of can heat in atmosphere without particle conductive copper ink, by copper presoma, complexing agent, solvent and
Auxiliary agent is obtained；Wherein, each component and its mass percent be, copper presoma：20~73%, complexing agent：15~60%, it is molten
Agent：10~51%, auxiliary agent：0~10%；
Described copper presoma be copper nitrate, cupric oxide, do not contain hydroxyl aliphatic carboxylic acid copper, aromatic carboxylic acid copper or
One or more mixing in alicyclic carboxylic acid copper；
Described complexing agent is with the one kind in 1~6 fatty amine of N atoms, hydramine, acid amides, aromatic amine, aliphatic cyclic amine
Or several mixing；
Described solvent is one or more mixing in water or alcohol compound；
Described auxiliary agent is polyethylene glycol, polyvinyl alcohol, polyethylene pyrrole network alkanone, polyacrylic acid, ammonium polyacrylate, poly- first
One or more mixing in base ammonium acrylate, Arabic gum, ethyl cellulose, hydroxymethyl cellulose, Span or tween.
Described Span is the one kind in Span 85, Span 80, Span 60, Span 40 or Span 20；
One kind in the polysorbate85 of described tween, Tween 80, polysorbate60, polysorbate40 or polysorbas20；
When described copper presoma is the mixture of several mixing, mixed proportion is any ratio.
When described complexing agent is the mixture of several mixing, mixed proportion is any ratio.
In described solvent, described alcohol compound be containing 1~3 hydroxy functional group and carbon atom number be 1~
12 alcohol compound.When described solvent is water, the copper-based conductive ink of agranular type need to add auxiliary agent.
When described auxiliary agent is the mixture of several mixing, mixed proportion is any ratio.
Described can heat in atmosphere is blueness without particle conductive copper ink, without any solid particle, ink viscosity
It is 1~1000mPas, contact angle is 15~65 °, and surface tension is 20~60mN/m, and 2 years are stored at room temperature without any face
Color change and precipitation generation.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, will be complexed
Agent adds auxiliary agent and solvent, is well mixed, and obtains mixed solution；
(2) to copper presoma in mixed solution, is added, stirring to copper presoma is all dissolved, was carried out with miillpore filter
Filter, be obtained can heat in atmosphere without particle conductive copper ink.
In described step (1), described is well mixed, and incorporation time is 15~30min.
In described step (2), described stirring, whipping temp is room temperature, and mixing time is 0.5~12h.
In described step (2), the aperture of described miillpore filter is 220nm or 450nm.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink or film are sintered in atmosphere on substrate, and sintering condition is：It is heated to 130~350
DEG C, 1~15min is heat-treated, the Copper thin film/copper conductor being bonded on substrate is obtained.
The resistivity of obtained Copper thin film/copper conductor is 4.1~56.7 μ Ω cm.The obtained copper being bonded on substrate
Film, with 3M, after 600M tape pulls, comes off without Copper thin film, and will not after the Copper thin film of flexible base board generation bends 200 times
Breakage, the ＜ R/R of resistivity ratio 10(wherein R is the resistivity of Copper thin film after bending every time, R to ＜ 2.50It is the resistance before bending
Rate).
In described application method, described substrate is PET (PET), polyethersulfone resin (PES),
It is a kind of in PEN (PEN), polyimides (PI), glass, monocrystalline silicon, quartz plate, potsherd or printing paper.
The preparation method without particle conductive copper ink that can be heated in atmosphere of the invention, in described step (2), copper
When presoma is added to mixed solution, there is following reaction：
Cu-R+4R’-NH2→Cu(R’-NH2)4R
Wherein, R represents copper nitrate, cupric oxide, do not contain hydroxyl aliphatic carboxylic acid copper, aromatic carboxylic acid copper or alicyclic
Other functional groups in copper carboxylate beyond copper removal, R ' represent there is 1-6 N atom fatty amine, hydramine, acid amides, aromatic amine or
Other functional groups in aliphatic cyclic amine in addition to amidine functional group.
It is of the invention it is a kind of can heat in atmosphere without particle conductive copper ink and its preparation and application, compared to
Prior art, its advantage is：
1. it is of the invention can heat in atmosphere without particle conductive copper ink, do not contain any solid particle, overcome biography
Intrinsic shortcoming (stability is low, sintering temperature is high) in system granular pattern copper ink, stability is high, and preparation method is simple to operation,
Solidification temperature is low, and the time is short, pollution-free, and good conductivity is with low cost, it is easy to accomplish industrialization.
2. it is of the invention can heat in atmosphere without particle conductive copper ink, regulation complex compound decomposition temperature is waved with solvent
Tandem between hair temperature, can in atmosphere sinter and obtain elemental copper, without in inert gas, reducibility gas and vacuum
Sintered under atmosphere, reduce dangerous and cost-effective and operating procedure.
3. after the present invention heat treatment Copper thin film resistivity that obtains in 4.1~56.7 μ Ω cm, with granular pattern and other nothings
Granular pattern sinters that the Copper thin film for obtaining is very nearly the same under inert gas or reducibility gas, and Copper thin film and substrate attachment
Property it is good, with 3M, come off without Copper thin film after 600M tape pulls, and after the Copper thin film of flexible base board generation bends 200 times not
Can be damaged, (wherein R is the resistivity of Copper thin film after bending every time to the ＜ R/R0 ＜ 2.5 of resistivity ratio 1, and R0 is the electricity before bending
Resistance rate).
4. it is of the invention can heat in atmosphere without particle conductive copper ink, viscosity is in 1~1000mPas, contact angle
It is 15~65 °, surface tension is 20~60mN/m, 2 years is stored at room temperature without any color change and precipitation generation.Additionally,
Various material can be used for using the conductive Copper thin film prepared without particle conductive copper ink that can be heated in atmosphere of the invention, such as
Plastics, silicon, glass, ceramics, paper etc., in applying also for various printing processes or various coating methods.Printing process, for example
Silk-screen printing, inkjet printing, intaglio printing, letterpress, flexible printing, offset printing etc.；Coating method, for example, scrape cutter painting
Cloth, silk rod coating, rotary coating, spraying, dip-coating etc..Wherein for printing process, ink of the range of viscosities in 1~20mPas
It is adapted to inkjet printing, and ink of the viscosity higher than 20mPas is adapted to the mode of printings such as silk-screen printing, flexible printing.
Brief description of the drawings
Fig. 1 is the XRD spectrum of Copper thin film in embodiment 1.
Fig. 2 is the SEM shape appearance figures of Copper thin film in embodiment 2.
Fig. 3 is the Cu 2p XPS figures of Copper thin film in embodiment 3.
Fig. 4 is the SEM shape appearance figures of Copper thin film in embodiment 4.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.
In following examples, using model LVDV-II+Pro, Brookfield Engineering Labs Inc.,
The viscosity without particle conductive copper ink that the viscosimeter test of USA can be heated in atmosphere, using section of the U.S. promise limited public affairs of industry
Contact angle without particle conductive copper ink and surface tension that department's SL200KS contact angle instruments measurement can be heated in atmosphere, use
The probe instrument of four 8 types of probe Science and Technology Ltd. RTS of Guangzhou four measures the resistivity of Copper thin film, using Japanese JEOL
Company JSM-700IF types field emission scanning electron microscope observes Copper thin film pattern, using the XploRA of Japanese Horiba companies
Laser co-focusing test system viewing Copper thin film surface in PLUS Raman spectrometers.
Embodiment 1
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper acetate, ethylenediamine, isopropanol and polyethylene glycol
It is obtained；Wherein, each component and its mass percent are that copper acetate is 35%, and ethylenediamine is 20%, and isopropanol is 43%, are gathered
Ethylene glycol is 2%；
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by second two
Amine solvent is well mixed in isopropanol and polyethylene glycol, and incorporation time is 15min, obtains mixed solution；
(2) to copper acetate in mixed solution, is added, 25 DEG C of stirring 2h all dissolve to copper acetate, are 220nm with aperture
Miillpore filter filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 12mPas, contact angle is 20 °, and surface tension is 35mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink jet is printed on PEN (PEN) substrate, is sintered in atmosphere, sintered bar
Part is：200 DEG C are heated to, 2min is heat-treated, the conductive copper conductor being bonded on PEN substrates, obtained conductive copper conductor is obtained
Resistivity be 10 μ Ω cm.
The XRD spectrum of obtained conductive Copper thin film is shown in Fig. 1, and its diffraction maximum is contrasted with JCPDS standard cards, its data result
With good.
Embodiment 2
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper formate, Isosorbide-5-Nitrae butanediamine, ethylene glycol and the third three
Alcohol is obtained；Wherein, each component and its mass percent are that copper formate is 20%, and Isosorbide-5-Nitrae butanediamine is 60%, and ethylene glycol is
15%, glycerine is 5%；
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by Isosorbide-5-Nitrae
Butanediamine is dissolved in ethylene glycol and glycerine, is well mixed, and incorporation time is 30min, obtains mixed solution；
(2) to copper formate in mixed solution, is added, 25 DEG C of stirring 10h all dissolve to copper formate, are 450nm with aperture
Miillpore filter filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 600mPas, contact angle is 55 ° on quartzy plate base, and surface tension is 52mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink rotary coating is sintered in atmosphere on quartzy plate base, and sintering condition is：300 DEG C are heated to,
Heat treatment 5min, is obtained the conductive Copper thin film being bonded on quartzy plate base, and the resistivity of obtained conductive Copper thin film is 4.1 μ
Ω·cm。
The SEM shape appearance figures of obtained conductive Copper thin film are shown in Fig. 2, visible in figure, closely coupled between each particle, form coherent
Conductive channel, it is finer and close.
Embodiment 3
It is a kind of can heat in atmosphere without particle conductive copper ink, by propionic acid copper, succinic acid copper, diethanol amine, 12
Alcohol and polyacrylic acid are obtained；Wherein, each component and its mass percent are that propionic acid copper is 15%, and succinic acid copper is 22%, two
Monoethanolamine is 30%, and lauryl alcohol is 28%, and polyacrylic acid is 5%；
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by diethyl
Hydramine is dissolved in lauryl alcohol and POLYPROPYLENE GLYCOL, is well mixed, and incorporation time is 30min, obtains mixed solution；
(2) to propionic acid copper and succinic acid copper in mixed solution, is added, 25 DEG C are stirred 12h, complete to propionic acid copper and succinic acid copper
Portion dissolve, filtered with the miillpore filter that aperture is 220nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 290mPas, the contact angle on monocrystalline silicon substrate is 40 °, and surface tension is 55mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink scraper for coating is sintered in atmosphere on monocrystalline silicon substrate, and sintering condition is：250 DEG C are heated to,
Heat treatment 1min, is obtained the conductive Copper thin film being bonded on monocrystalline silicon substrate, and the resistivity of obtained conductive Copper thin film is 21 μ
Ω·cm。
The obtained Copper thin film being bonded on substrate, with 3M, after 600M tape pulls, comes off without Copper thin film, and in flexibility
The Copper thin film of substrate generation will not be damaged after bending 200 times, resistivity ratio R/R0It is 2.
The Cu 2p XPS figures of obtained conductive Copper thin film are shown in Fig. 3, have no Cu2+Peak position, and Cu 2p2/3Correspond in 932eV,
It is elemental copper.
Embodiment 4
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper benzoate, propane diamine, methyl alcohol, water, penta 2
Alcohol, polyethylene glycol and polyethylene pyrrole network alkanone are obtained；Wherein, each component and its mass percent are that copper benzoate is 25%,
Propane diamine is 17%, and methyl alcohol is 13%, and water is 16%, and pentanediol is 19%, and polyethylene glycol is 3%, and polyethylene pyrrole network alkanone is
7%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by the third two
Amine solvent in polyethylene glycol and polyethylene pyrrole network alkanone, is well mixed in methyl alcohol, water, pentanediol, and incorporation time is 20min, is obtained
To mixed solution；
(2) in mixed solution, adding copper benzoate, 25 DEG C of stirring 6h all to be dissolved to copper benzoate, it is with aperture
The miillpore filter of 450nm is filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 15mPas, contact angle on the glass substrate is 15 °, and surface tension is 31mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper emitting ink is sintered in atmosphere on glass substrate, and sintering condition is：It is heated to 190 DEG C, heat treatment
15min, prepared bonding conductive Copper thin film on the glass substrate, the resistivity of obtained conductive Copper thin film is 26 μ Ω cm.
The SEM shape appearance figures of obtained Copper thin film are shown in Fig. 4, and film is more smooth, and continuous conduction passage is formed between copper particle.
Embodiment 5
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper formate, copper acetate, ethylenediamine, ethanol and second
Glycol is obtained；Wherein, each component and its mass percent are that copper formate is 12%, and copper acetate is 13%, and ethylenediamine is
47%, ethanol is 14%, and ethylene glycol is 14%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by second two
Amine solvent is well mixed in ethanol and ethylene glycol, and incorporation time is 20min, obtains mixed solution；
(2) to copper formate and copper acetate in mixed solution, is added, 25 DEG C are stirred 0.5h, to copper formate and copper acetate whole
Dissolving, filtered with the miillpore filter that aperture is 220nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 5mPas, the contact angle on pet substrate is 22 °, and surface tension is 28mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink flat board is printed on pet substrate, is sintered in atmosphere, and sintering condition is：It is heated to 130 DEG C, heat
Treatment 8min, is obtained the conductive Copper thin film being bonded on pet substrate, and the resistivity of obtained conductive Copper thin film is 46 μ Ω cm.
Embodiment 6
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper nitrate, copper acetate, triethylene tetramine, enanthol
It is obtained with Span 80；Wherein, each component and its mass percent are that copper nitrate is 27%, and copper acetate is 11%, triethylene four
Amine is 31%, and enanthol is 24%, and Span 80 is 7%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by three second
Alkene tetramine is dissolved in enanthol and Span 80, is well mixed, and incorporation time is 20min, obtains mixed solution；
(2) to copper nitrate and copper acetate in mixed solution, is added, 25 DEG C are stirred 2h, all molten to copper nitrate and copper acetate
Solution, filtered with the miillpore filter that aperture is 220nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 8mPas, the contact angle on polyimides (PI) substrate is 29 °, and surface tension is 35mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink filaments rod film is sintered in atmosphere on PI substrates, and sintering condition is：It is heated to 270 DEG C, at heat
Reason 2min, is obtained the conductive Copper thin film being bonded on PI substrates, and the resistivity of obtained conductive Copper thin film is 22 μ Ω cm.
Embodiment 7
It is a kind of can heat in atmosphere without particle conductive copper ink, by cupric oxide, oleyl amine, ethohexadiol, butenol, Span
80 and polyethylene glycol be obtained；Wherein, each component and its mass percent are that cupric oxide is 30%, and oleyl amine is 32%, ethohexadiol
It is 21%, butenol is 13%, Span 80 is 1%, and polyethylene glycol is 3%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by oleyl amine
Ethohexadiol is dissolved in, butenol in Span 80 and polyethylene glycol, is well mixed, and incorporation time is 30min, obtains mixed solution；
(2) to cupric oxide in mixed solution, is added, 25 DEG C of stirring 11h all dissolve to cupric oxide, are 450nm with aperture
Miillpore filter filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 12mPas, the contact angle on monocrystalline silicon substrate is 49 °, and surface tension is 42mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink dip-coating is sintered in atmosphere on monocrystalline silicon substrate, and sintering condition is：It is heated to 350 DEG C, at heat
Reason 15min, is obtained the conductive Copper thin film being bonded on monocrystalline silicon substrate, and the resistivity of obtained conductive Copper thin film is 15 μ Ω
cm。
Embodiment 8
It is a kind of can heat in atmosphere without particle conductive copper ink, by malonic acid copper, aniline, triethanolamine, certain herbaceous plants with big flowers alcohol, third
Triol and Arabic gum are obtained；Wherein, each component and its mass percent are that malonic acid copper is 35%, and aniline is 9%, three
Monoethanolamine is 21%, and certain herbaceous plants with big flowers alcohol is 10%, and glycerine is 19%, and Arabic gum is 6%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by aniline
Certain herbaceous plants with big flowers alcohol is dissolved in triethanolamine, in glycerine and Arabic gum, is well mixed, incorporation time is 30min, obtains mixing molten
Liquid；
(2) in mixed solution, adding malonic acid copper, 25 DEG C of stirring 6h all to be dissolved to malonic acid copper, it is with aperture
The miillpore filter of 450nm is filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 1000mPas, the contact angle on aluminium oxide ceramics plate base is 65 °, and surface tension is 60mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink silk-screen printing is sintered in atmosphere on aluminium oxide ceramics plate base, and sintering condition is：It is heated to
330 DEG C, 5min is heat-treated, the conductive copper conductor being bonded on aluminium oxide ceramics plate base is obtained, obtained conductive copper conductor
Resistivity is 4.1 μ Ω cm.
Embodiment 9
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper stearate, tetraacetyl ethylene diamine, hexylamine, second
Glycol, butanol, POLYPROPYLENE GLYCOL and ethyl cellulose are obtained；Wherein, each component and its mass percent are that copper stearate is
73%, tetraacetyl ethylene diamine is 2%, and hexylamine is 13%, and ethylene glycol is 5%, and butanol is 5%, and POLYPROPYLENE GLYCOL is 1%, and ethyl is fine
Dimension element is 1%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by tetrem
Acyl ethylenediamine and hexylamine are dissolved in ethylene glycol, and butanol in polyvinyl alcohol and ethyl cellulose, is well mixed, and incorporation time is
30min, obtains mixed solution；
(2) in mixed solution, adding copper stearate, 25 DEG C of stirring 9h all to be dissolved to copper stearate, it is with aperture
The miillpore filter of 450nm is filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 70mPas, contact angle on the glass substrate is 43 °, and surface tension is 38mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink intaglio printing is sintered in atmosphere on glass substrate, and sintering condition is：It is heated to 270 DEG C, heat
Treatment 1min, prepared bonding conductive copper conductor on the glass substrate, the resistivity of obtained conductive copper conductor is 56.7 μ Ω
cm。
Embodiment 10
It is a kind of can heat in atmosphere without particle conductive copper ink, by cyclobutyl formate copper, TEPA, octanol,
Butanol and Tween 80 are obtained；Wherein, each component and its mass percent are that cyclobutyl formate copper is 30%, TEPA
It is 18%, octanol is 26%, butanol is 19%, Tween 80 is 7%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by tetrem
The amine solvent of alkene five is well mixed in octanol, butanol and Tween 80, and incorporation time is 20min, obtains mixed solution；
(2) to cyclobutyl formate copper in mixed solution, is added, 25 DEG C are stirred 3h, are all dissolved to cyclobutyl formate copper, are used
Aperture is filtered for the miillpore filter of 220nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 117mPas, the contact angle on silicon nitride ceramics plate base is 48 °, and surface tension is 41mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink flexible printing is sintered in atmosphere on silicon nitride ceramics plate base, and sintering condition is：It is heated to
340 DEG C, 3min is heat-treated, the conductive copper conductor being bonded on silicon nitride ceramics plate base is obtained, obtained conductive copper conductor
Resistivity is 16.1 μ Ω cm.
Embodiment 11
It is a kind of can heat in atmosphere without particle conductive copper ink, by cupric oxalate, tert-butylamine, cyclohexanediamine, ethylene glycol,
Methyl alcohol and ammonium polyacrylate are obtained；Wherein, each component and its mass percent are that cupric oxalate is 22%, and tert-butylamine is 10%,
Cyclohexanediamine is 16%, and ethylene glycol is 12%, and methyl alcohol is 39%, and ammonium polyacrylate is 1%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by tertiary fourth
Amine and cyclohexanediamine are dissolved in ethylene glycol, in methyl alcohol and ammonium polyacrylate, are well mixed, and incorporation time is 15min, is mixed
Solution；
(2) to cupric oxalate in mixed solution, is added, 25 DEG C of stirring 2h all dissolve to cupric oxalate, are 220nm with aperture
Miillpore filter filtered, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 18mPas, the contact angle on polyethersulfone resin (PES) substrate is 29 °, and surface tension is 31mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink jet is printed on PES substrates, is sintered in atmosphere, and sintering condition is：It is heated to 160 DEG C, heat
Treatment 6min, is obtained the conductive copper conductor being bonded on PES substrates, and the resistivity of obtained conductive copper conductor is 18.6 μ Ω
cm。
Embodiment 12
It is a kind of can heat in atmosphere without particle conductive copper ink, by cupric oxalate, propionic acid copper, isopropylamine, five ethene six
Amine, butanediol and ammonium polymethacrylate are obtained；Wherein, each component and its mass percent are that cupric oxalate is 10%, propionic acid
Copper is 13%, and isopropylamine is 26%, and pentaethylene hexamine is 14%, and butanediol is 35%, and ammonium polymethacrylate is 2%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by isopropyl
Amine and pentaethylene hexamine are dissolved in butanediol and ammonium polymethacrylate, are well mixed, and incorporation time is 15min, is mixed
Close solution；
(2) to cupric oxalate and propionic acid copper in mixed solution, is added, 25 DEG C are stirred 5h, all molten to cupric oxalate and propionic acid copper
Solution, filtered with the miillpore filter that aperture is 220nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 35mPas, the contact angle on PI substrates is 33 °, and surface tension is 37mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink intaglio printing is sintered in atmosphere on PI substrates, and sintering condition is：It is heated to 350 DEG C, at heat
Reason 15min, is obtained the conductive copper conductor being bonded on PI substrates, and the resistivity of obtained conductive copper conductor is 31.3 μ Ω cm.
Embodiment 13
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper nitrate, malonic acid copper, tert-butylamine, butanediamine,
Ethanol, ethylene glycol and hydroxymethyl cellulose are obtained；Wherein, each component and its mass percent are that copper nitrate is 20%, the third two
Sour copper is 23%, and tert-butylamine is 16%, and butanediamine is 11%, and ethanol is 20%, and ethylene glycol is 6%, and hydroxymethyl cellulose is
4%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by tertiary fourth
Amine and butanediamine are dissolved in ethanol, in ethylene glycol and hydroxymethyl cellulose, are well mixed, and incorporation time is 10min, is mixed
Solution；
(2) to copper nitrate and malonic acid copper in mixed solution, is added, 25 DEG C are stirred 4h, complete to copper nitrate and malonic acid copper
Portion dissolve, filtered with the miillpore filter that aperture is 450nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 40mPas, the contact angle on quartzy plate base is 38 °, and surface tension is 29mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink intaglio printing is sintered in atmosphere on quartzy plate base, and sintering condition is：230 DEG C are heated to,
Heat treatment 5min, is obtained the conductive copper conductor being bonded on quartzy plate base, and the resistivity of obtained conductive copper conductor is 23.8 μ
Ω·cm。
Embodiment 14
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper formate, cyclopenta copper formate, aniline, butylamine,
Water, isopropanol and polyethylene glycol are obtained；Wherein, each component and its mass percent are that copper formate is 18%, cyclopenta formic acid
Copper is 5%, and aniline is 6%, and butylamine is 28%, and water is 10%, and isopropanol is 26%, and polyethylene glycol is 7%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by aniline
Water is dissolved in butylamine, in isopropanol and polyethylene glycol, is well mixed, incorporation time is 10min, obtains mixed solution；
(2) to copper formate and cyclopenta copper formate in mixed solution, is added, 25 DEG C are stirred 8h, to copper formate and cyclopenta
Copper formate all dissolves, and is filtered with the miillpore filter that aperture is 450nm, and can heat in atmosphere conductive without particle is obtained
Copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 94mPas, the contact angle on quartzy plate base is 34 °, and surface tension is 60mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink letterpress is sintered in atmosphere on quartzy plate base, and sintering condition is：200 DEG C are heated to,
Heat treatment 3min, is obtained the conductive Copper thin film being bonded on quartzy plate base, and the resistivity of obtained conductive Copper thin film is 38.5 μ
Ω·cm。
Embodiment 15
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper formate, copper acetate, butanediamine, nonyl alcohol and poly-
Vinyl alcohol is obtained；Wherein, each component and its mass percent are that copper formate is 34%, and copper acetate is 6%, and butanediamine is
30%, nonyl alcohol is 28%, and polyvinyl alcohol is 2%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by fourth two
Amine solvent is well mixed in nonyl alcohol and polyvinyl alcohol, and incorporation time is 15min, obtains mixed solution；
(2) to copper formate and copper acetate in mixed solution, is added, 25 DEG C are stirred 5h, all molten to copper formate and copper acetate
Solution, filtered with the miillpore filter that aperture is 450nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 31mPas, the contact angle on phase paper base plate is 31 °, and surface tension is 38mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper solid ink is applied on phase paper base plate, is sintered in atmosphere, and sintering condition is：It is heated to 220 DEG C, heat treatment
6min, is obtained the conductive Copper thin film being bonded on phase paper base plate, and the resistivity of obtained conductive Copper thin film is 7.8 μ Ω cm.
Embodiment 16
It is a kind of can heat in atmosphere without particle conductive copper ink, by copper formate, copper acetate, butanediamine, nonyl alcohol and poly-
Vinyl alcohol is obtained；Wherein, each component and its mass percent are that copper formate is 34%, and copper acetate is 6%, and butanediamine is
30%, nonyl alcohol is 28%, and polyvinyl alcohol is 2%.
A kind of preparation method without particle conductive copper ink that can be heated in atmosphere, comprises the following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, each component is weighed, by fourth two
Amine solvent is well mixed in nonyl alcohol and polyvinyl alcohol, and incorporation time is 25min, obtains mixed solution；
(2) to copper formate and copper acetate in mixed solution, is added, 25 DEG C are stirred 0.5h, to copper formate and copper acetate whole
Dissolving, filtered with the miillpore filter that aperture is 450nm, be obtained can heat in atmosphere without particle conductive copper ink.
It is obtained can heat in atmosphere without particle conductive copper ink for blueness, without any solid particle, ink viscosity
It is 1mPas, the contact angle on phase paper base plate is 15 °, and surface tension is 20mN/m.
A kind of application method without particle conductive copper ink that can heat in atmosphere is：The nothing that be able to will be heated in atmosphere
Particle conductive copper ink jet is printed on phase paper base plate, is sintered in atmosphere, and sintering condition is：It is heated to 170 DEG C, heat
Treatment 6min, is obtained the Copper thin film being bonded on phase paper base plate, and the resistivity of obtained Copper thin film is 7.8 μ Ω cm.
Claims (10)
1. it is a kind of can heat in atmosphere without particle conductive copper ink, it is characterised in that the nothing that can be heated in atmosphere
Grain conductive copper ink is obtained by copper presoma, complexing agent, solvent and auxiliary agent；Wherein, each component and its mass percent be, copper
Presoma：20~73%, complexing agent：15~60%, solvent：10~51%, auxiliary agent：0~10%；
Aliphatic carboxylic acid copper, aromatic carboxylic acid copper or alicyclic ring that described copper presoma is copper nitrate, cupric oxide, does not contain hydroxyl
One or more mixing in race's copper carboxylate；
Described complexing agent is with the one kind or several in 1~6 fatty amine of N atoms, hydramine, acid amides, aromatic amine, aliphatic cyclic amine
Plant mixing；
Described solvent is one or more mixing in water or alcohol compound；
Described auxiliary agent is polyethylene glycol, polyvinyl alcohol, polyethylene pyrrole network alkanone, polyacrylic acid, ammonium polyacrylate, poly- methyl-prop
One or more mixing in olefin(e) acid ammonium, Arabic gum, ethyl cellulose, hydroxymethyl cellulose, Span or tween.
2. can heat in atmosphere as claimed in claim 1 without particle conductive copper ink, it is characterised in that described solvent
In, described alcohol compound is to contain the alcohol compound that 1~3 hydroxy functional group and carbon atom number are 1~12；It is described
Solvent be water when, the copper-based conductive ink of agranular type need to add auxiliary agent.
3. can heat in atmosphere as claimed in claim 1 without particle conductive copper ink, it is characterised in that described auxiliary agent
In, described Span is the one kind in Span 85, Span 80, Span 60, Span 40 or Span 20；The tween of described tween
85th, one kind in Tween 80, polysorbate60, polysorbate40 or polysorbas20.
4. can heat in atmosphere as claimed in claim 1 without particle conductive copper ink, it is characterised in that it is described can be
It is blueness without particle conductive copper ink to be heated in air, and without any solid particle, ink viscosity is 1~1000mPas, is connect
Feeler is 15~65 °, and surface tension is 20~60mN/m.
5. the preparation method without particle conductive copper ink that can be heated in atmosphere described in claim 1, it is characterised in that bag
Include following steps：
(1) according to the component proportion without particle conductive copper ink that can be heated in atmosphere, weigh each component, by complexing agent plus
Enter auxiliary agent and solvent, be well mixed, obtain mixed solution；
(2) to copper presoma in mixed solution, is added, stirring to copper presoma is all dissolved, is filtered with miillpore filter, is made
Can heat in atmosphere without particle conductive copper ink.
6. the preparation method without particle conductive copper ink that can be heated in atmosphere as claimed in claim 5, it is characterised in that
In described step (1), described is well mixed, and incorporation time is 15~30min.
7. the preparation method without particle conductive copper ink that can be heated in atmosphere as claimed in claim 5, it is characterised in that
In described step (2), described stirring, whipping temp is room temperature, and mixing time is 0.5~12h；In described step (2),
The aperture of described miillpore filter is 220nm or 450nm.
8. the application method without particle conductive copper ink that can be heated in atmosphere described in claim 1, it is characterised in that should
The application method without particle conductive copper ink that can be heated in atmosphere is：Be able to will heat in atmosphere without particle conductive copper ink
Printing stock or film are sintered in atmosphere on substrate, and sintering condition is：It is heated to 130~350 DEG C, heat treatment 1~
15min, is obtained the Copper thin film being bonded on substrate or the copper conductor being bonded on substrate.
9. the application method without particle conductive copper ink that can be heated in atmosphere as claimed in claim 8, it is characterised in that
Described Copper thin film or the resistivity of copper conductor are 4.1~56.7 μ Ω cm；The obtained Copper thin film being bonded on substrate, uses
After 3M, 600M tape pull, come off without Copper thin film, and will not be damaged after the Copper thin film of flexible base board generation bends 200 times, electricity
The ＜ R/R of resistance rate ratio 10＜ 2.5.
10. the application method without particle conductive copper ink that can be heated in atmosphere as claimed in claim 8, its feature exists
In in described application method, described substrate is PET, polyethersulfone resin, poly- naphthalenedicarboxylic acid second two
It is a kind of in alcohol ester, polyimides, glass, monocrystalline silicon, quartz plate, potsherd or printing paper.
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| CN107778995A (en) * | 2017-11-16 | 2018-03-09 | 辽宁大学 | A kind of copper-based conductive ink of high stability agranular type containing copper formate and its preparation method and application |
| CN108566735A (en) * | 2017-12-15 | 2018-09-21 | 中国科学院福建物质结构研究所 | A kind of array Cu oxide semiconductor transducer and its preparation method and application |
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| JP2021533229A (en) * | 2018-08-03 | 2021-12-02 | ナショナル リサーチ カウンシル オブ カナダ | UV sinterable molecular ink using wide-spectrum UV light and its treatment |
| JP7374177B2 (en) | 2018-08-03 | 2023-11-06 | ナショナル リサーチ カウンシル オブ カナダ | UV sinterable molecular ink and its processing using broad spectrum UV light |
| US11873413B2 (en) | 2018-08-03 | 2024-01-16 | National Research Council Of Canada | UV-sinterable molecular ink and processing thereof using broad spectrum UV light |
| CN110186986A (en) * | 2019-06-21 | 2019-08-30 | 福建工程学院 | Electrochemical glucose sensor and its detection method without enzyme |
| CN111269615A (en) * | 2020-03-20 | 2020-06-12 | 辽宁大学 | Antioxidant particle-free copper conductive ink and preparation method thereof |
| CN116285503A (en) * | 2023-03-14 | 2023-06-23 | 广东电网有限责任公司 | Particle-free copper conductive ink and conductive copper film for 3D ink-jet printing and preparation methods thereof |
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