CN106147407A - A kind of Graphene water color ink of high connductivity - Google Patents
A kind of Graphene water color ink of high connductivity Download PDFInfo
- Publication number
- CN106147407A CN106147407A CN201610841641.9A CN201610841641A CN106147407A CN 106147407 A CN106147407 A CN 106147407A CN 201610841641 A CN201610841641 A CN 201610841641A CN 106147407 A CN106147407 A CN 106147407A
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- graphene
- color ink
- water
- copper powder
- high connductivity
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The invention provides the Graphene water color ink of a kind of high connductivity, this ink uses following methods to prepare: prepared by superfine cupper powder, weighing of raw material: weigh each raw material according to following mass percent: copper powder 5～8%, Graphene 55～62%, acrylic resin 5～9%, alkyd resin 2～4%, acetate butyl 7～11%, deionized water 7～11%, defoamer 0.2～2%, levelling agent 0.2～2%, water-based thickener 2～4%；Raw material stirring；Grind.The Graphene water color ink resistivity of obtained high connductivity is not more than 1.2 × 10‑3Ω cm, using cross-hatching to test its adhesive force is more than 98%.Graphene and superfine cupper powder are combined as a kind of complex conductive fillers medium by this ink, i.e. reduce cost, have again high conductivity and oxygen-proof property, and meanwhile, this ink uses water and alcohol to replace conventional organic solvents, also has environmental protection, nontoxic advantage.
Description
Technical field
The invention provides a kind of water color ink, particularly provide a kind of Graphene water color ink with high conductivity,
Belong to printing technology.
Background technology
Along with developing rapidly of nanotechnology, the electrically conductive ink of Nano grade is by the high speed industrialization of printed electronics
At home and abroad receive much concern.And water color ink uses water to replace organic solvent, there is VOC nontoxic, low and the environmental protection such as non-combustible is special
Point, is just becoming the main flow of 21 century printing industry Green Development.
Water-soluble conducting ink, as the term suggests being exactly the ink being combined with water color ink Dominant Facies by electric conductivity.At present, complete
Complete utilization Graphene is as the ink of conducting medium, relatively costly；And if only utilizing the less expensive metal dusts such as copper powder
If conducting medium, although cost is relatively low, but copper powder is oxidized easily, and electric conductivity is highly unstable.Therefore, find
The water color ink that a kind of cost and electric conductivity are taken into account meets demand and the developing direction of ink research of society.
Summary of the invention
The invention provides the Graphene water color ink of a kind of high connductivity, solve the deficiency in background technology, this ink
Graphene and superfine cupper powder are combined as a kind of complex conductive fillers medium, i.e. reduce cost, have again high conductivity and
Oxygen-proof property, meanwhile, this ink uses water and alcohol to replace conventional organic solvents, also has environmental protection, nontoxic advantage.
Realizing the technical scheme that above-mentioned purpose of the present invention used is:
The Graphene water color ink of a kind of high connductivity, this ink uses following methods to prepare: prepared by (1) superfine cupper powder: will
Schweinfurt green joins in polyhydric alcohol, adds ammonia under keeping 60～70 DEG C of bath temperatures, prepares blueness after abundant complex reaction
Copper ammon solution；It is that 5%～10% hydrazine hydrate solution is the most dropwise slowly dropped in copper ammon solution by volume fraction,
By reactant mixture centrifugation after dropping, obtain aubergine powder and be product copper powder；After copper powder washing, prepare
The mixture of copper powder and water, prepare a diameter of the 50～500nm of copper powder；
(2) the weighing of raw material: weigh each raw material according to following mass percent: copper powder 5～8%, Graphene 55～62%,
Acrylic resin 5～9%, alkyd resin 2～4%, acetate butyl 7～11%, deionized water 7～11%, defoamer 0.2～
2%, levelling agent 0.2～2%, water-based thickener 2～4%；
(3) raw material stirring: alkyd resin and acrylic resin, deionized water, ethanol are put into and fully stir to Scattered Kettle
Mixing, temperature is set to 30～40 DEG C, and controlling mixing speed is 400～500rpm；The most again by Graphene, copper powder, aqueous thickening
Agent, levelling agent, defoamer stir in putting into Scattered Kettle, and temperature is set to 30～40 DEG C, control mixing speed and are
400～500rpm；
(4) grind: be ground in scattered material is moved to grinder, be fully ground until the fineness of material reaches
Below 15 μm, can be prepared by the Graphene water color ink of high connductivity.
Polyhydric alcohol described in step (1) is ethylene glycol, diglycol or glycerol.
In step (1), first with copper powder being washed with deionized 2～3 times, then with the ethanol solution of BTA
Wash 1～2 time.
The Graphene water color ink resistivity of high connductivity obtained in step (4) is not more than 1.2 × 10-3Ω cm, adopts
Testing its adhesive force with cross-hatching is more than 98%.
Owing to superfine cupper powder is the most oxidized, therefore the present invention is during preparing superfine cupper powder, using polyhydric alcohol as
Solvent, the reproducibility of polyhydric alcohol itself can prevent reduzate oxidized, and its viscosity is conducive to the granule that dispersion generates, polyhydric alcohol
Separate from reaction system with the good solubility dissolved each other the beneficially pressed powder of water.Washing process utilizes containing phenylpropyl alcohol three
The ethanol solution washed product copper powder of nitrogen azoles, it is possible to form multilayer resist on copper surface, makes copper surface not play oxidation also
Former reaction.Hydrazine hydrate can not only reduce copper as the efficient reducing agent of one from mantoquita, itself reproducibility and also
The copper generated can be played the protective effect of anti-oxidation by the nitrogen that former reaction generates.Therefore present invention energy in preparation technology
Superfine cupper powder obtained by enough guarantees is not oxidized.
Compared with prior art, the Graphene water color ink of high connductivity provided by the present invention have the advantage that 1, this
In ink prepared by invention, owing to graphene carbon carbon bond is only 1.42Å, therefore structure is highly stable.Graphene only belongs to
In nanoscale, the thickness of single-layer graphene is about 0.334nm, and Graphene relies primarily on stirring with the mixing and absorption process of copper powder
Carry out, make Graphene gradually be adsorbed in Copper Powder Surface during stirring, owing to copper powder quality is relatively big relative to Graphene,
Sink under the effect of gravity, and be divided into upper and lower two-layer under gravity；And Graphene is little due to light weight, volume, it is inhaled
The upper surface being attached to copper powder particle forms one layer of extremely thin protecting film, effectively prevents the oxidation of copper powder.Added simultaneously
Thickening agent makes solution denseness bigger so that conductive filler (Graphene+copper powder) is suspended in ink mixture, will not be the most heavy
Fall.Therefore the ink not only electric conductivity that the present invention provides is good, it is crucial that production cost is greatly reduced.2, this
The organic solvents such as original benzene class are provided with water and alcohol in the ink of bright offer, greatly reduce organic volatile and arrange
Put, safety and environmental protection, the environment-friendly type printing material being well recognized as.It is applicable to the packaging that the security requirement such as food, medicine is higher.3, originally
The water color ink production cost of the superelevation conduction that invention provides is low, technique simple, can prepare in a large number, is suitable for industry metaplasia
Produce, and electric conductivity is superior, therefore, it is possible at electronics such as radio-frequency recognition system, intelligent packaging, conducting wire and sensors
Product is extensively applied, there is important practical significance and huge economic worth.
Detailed description of the invention
Below in conjunction with specific embodiment the present invention done detailed specific description, but protection scope of the present invention not office
It is limited to following example.
Embodiment 1
One: reduction copper ion, utilize polyol reduction method to prepare superfine cupper powder
1) weigh a certain amount of Schweinfurt green and join in 100ml ethylene glycol, add appropriate at keeping bath temperature 60 DEG C
Itself and the abundant complexation of copper powder is made to obtain blue copper ammon solution during ammonia.
2) 8ml hydrazine hydrate is diluted to volume fraction for 6% with deionized water, is the most dropwise slowly dropped to
In copper ammon solution.By reactant mixture centrifugation after dropping, obtain aubergine powder and be reduzate copper；
3) product copper is washed 1 time with the ethanol solution of deionized water wash 2 times, BTA, the copper prepared
Powder is with the mixture of water, and the solid content of copper powder is 90%, prepares the average diameter of copper powder all at about 200nm.
The proportioning of the most each raw material is as shown in the table:
Two: prepare Graphene～carbon system water color ink that copper powder compounded material is conductive filler.
1), needed for according to formula, alkyd resin and acrylic acid mixed resin liquid, deionized water, ethanol are put in Scattered Kettle
Being sufficiently stirred for, temperature is set to 30 DEG C, and control mixing speed is 400rpm.
2), needed for pressing formula, claim meta anthracite alkene, superfine cupper powder, thickening agent, levelling agent, defoamer etc. and put into Scattered Kettle
Inside stirring, temperature is set to 30 DEG C, and control mixing speed is 400rpm.
3) it is ground in scattered material being moved to grinder, grinds 2h, measure fineness and reach below 15 μm.
Otherwise continue to grind, until fineness reaches requirement.
Mass percent shared by each raw material and each raw material is as shown in the table:
Produced above for former ink, need before use to be diluted, the mixing using deionized water and ethanol during dilution is molten
Liquid, the ammonia utilizing content to be 5% regulation pH value is between 8～9.
The performance indications of ink obtained in the present embodiment are as shown in the table
| Conductive particle fineness/nm | Adhesive force (cross-hatching) | Resistivity/Ω cm | Dried film thickness/μm |
| ≤300 | >=98% | ≤1.2×10-3 | 10 |
Embodiment 2
One: reduction copper ion, utilize polyol reduction method to prepare superfine cupper powder
Weigh a certain amount of Schweinfurt green and join in 100ml glycerol, at keeping bath temperature 70 DEG C, add appropriate amounts of ammonia
Itself and the abundant complexation of copper powder is made to obtain blue copper ammon solution during water.
11ml hydrazine hydrate is diluted to volume fraction for 9% with deionized water, is the most dropwise slowly dropped to
In copper ammon solution.By reactant mixture centrifugation after dropping, obtain aubergine powder and be reduzate copper；
Product copper is washed 2 times with the ethanol solution of deionized water wash 3 times, BTA, the copper powder prepared
With the mixture of water, the solid content of copper powder is 90%, prepares the average diameter of copper powder all at about 300nm.
The proportioning of the most each raw material is as shown in the table:
Two: prepare Graphene～carbon system water color ink that copper powder compounded material is conductive filler.
Needed for formula, fill in alkyd resin and acrylic acid mixed resin liquid, deionized water, ethanol are put into Scattered Kettle
Dividing stirring, temperature is set to 40 DEG C, and control mixing speed is 500rpm.
Needed for formula, claim meta anthracite alkene, superfine cupper powder, thickening agent, levelling agent, defoamer etc. and put in Scattered Kettle
Stirring, temperature is set to 40 DEG C, and control mixing speed is 500rpm.
It is ground in scattered material is moved to grinder, grinds 2h, measure fineness and reach below 15 μm.No
Then continue to grind, until fineness reaches requirement.
Mass percent shared by each raw material and each raw material is as shown in the table:
Claims (4)
1. the Graphene water color ink of a high connductivity, it is characterised in that this ink uses following methods to prepare: (1) superfine cupper powder
Preparation: joined by Schweinfurt green in polyhydric alcohol, adds ammonia under keeping 60～70 DEG C of bath temperatures, makes after abundant complex reaction
Obtain blue copper ammon solution；It is that 5%～10% hydrazine hydrate solution is the most dropwise slowly dropped to cuprammonium by volume fraction
In solution, by reactant mixture centrifugation after dropping, obtain aubergine powder and be product copper powder；By copper powder washing
After, the copper powder prepared and the mixture of water, prepare a diameter of the 50～500nm of copper powder；
(2) the weighing of raw material: weigh each raw material according to following mass percent: copper powder 5～8%, Graphene 55～62%, propylene
Acid resin 5～9%, alkyd resin 2～4%, acetate butyl 7～11%, deionized water 7～11%, defoamer 0.2～2%, stream
Flat agent 0.2～2%, water-based thickener 2～4%；
(3) raw material stirring: alkyd resin and acrylic resin, deionized water, ethanol are put into and be sufficiently stirred for Scattered Kettle, temperature
Degree is set to 30～40 DEG C, and controlling mixing speed is 400～500rpm；The most again by Graphene, copper powder, water-based thickener, stream
Flat agent, defoamer stir in putting into Scattered Kettle, and temperature is set to 30～40 DEG C, control mixing speed be 400～
500rpm；
(4) grind: be ground in scattered material is moved to grinder, be fully ground until the fineness of material reaches 15 μm
Hereinafter, can be prepared by the Graphene water color ink of high connductivity.
The Graphene water color ink of high connductivity the most according to claim 1, it is characterised in that: many described in step (1)
Unit's alcohol is ethylene glycol, diglycol or glycerol.
The Graphene water color ink of high connductivity the most according to claim 1, it is characterised in that: in step (1), first with by copper
Powder is washed with deionized 2～3 times, then washs 1～2 time with the ethanol solution of BTA.
The Graphene water color ink of high connductivity the most according to claim 1, it is characterised in that: obtained by step (4)
The Graphene water color ink resistivity of high connductivity is not more than 1.2 × 10-3Ω cm, using cross-hatching to test its adhesive force is 98%
Above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610841641.9A CN106147407A (en) | 2016-09-22 | 2016-09-22 | A kind of Graphene water color ink of high connductivity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610841641.9A CN106147407A (en) | 2016-09-22 | 2016-09-22 | A kind of Graphene water color ink of high connductivity |
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| CN106147407A true CN106147407A (en) | 2016-11-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111849253A (en) * | 2020-08-07 | 2020-10-30 | 河南墨特石墨烯科技有限公司 | Graphene heating water-based ink and preparation method thereof |
| CN112276077A (en) * | 2020-10-28 | 2021-01-29 | 福州市辰亿五金制品有限公司 | High-wear-resistance copper-coated graphite for oil-retaining bearing and manufacturing method thereof |
Citations (3)
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|---|---|---|---|---|
| CN103073953A (en) * | 2013-02-07 | 2013-05-01 | 苏州牛剑新材料有限公司 | Waterborne conductive ink and preparation method thereof |
| CN103769598A (en) * | 2013-10-08 | 2014-05-07 | 东江环保股份有限公司 | Method for stably preparing nano-copper powder |
| CN104292983A (en) * | 2013-07-19 | 2015-01-21 | 海门市海菱碳业有限公司 | Conductive printing ink |
-
2016
- 2016-09-22 CN CN201610841641.9A patent/CN106147407A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073953A (en) * | 2013-02-07 | 2013-05-01 | 苏州牛剑新材料有限公司 | Waterborne conductive ink and preparation method thereof |
| CN104292983A (en) * | 2013-07-19 | 2015-01-21 | 海门市海菱碳业有限公司 | Conductive printing ink |
| CN103769598A (en) * | 2013-10-08 | 2014-05-07 | 东江环保股份有限公司 | Method for stably preparing nano-copper powder |
Non-Patent Citations (1)
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| 杨颖: "印刷电子用铜、银导电油墨的制备及性能研究", 《中国优秀硕士学位论文全文数据库（电子期刊），工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111849253A (en) * | 2020-08-07 | 2020-10-30 | 河南墨特石墨烯科技有限公司 | Graphene heating water-based ink and preparation method thereof |
| CN112276077A (en) * | 2020-10-28 | 2021-01-29 | 福州市辰亿五金制品有限公司 | High-wear-resistance copper-coated graphite for oil-retaining bearing and manufacturing method thereof |
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Application publication date: 20161123 |
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