CN105754416A - Preparation method of conductive ink - Google Patents
Preparation method of conductive ink Download PDFInfo
- Publication number
- CN105754416A CN105754416A CN201610310793.6A CN201610310793A CN105754416A CN 105754416 A CN105754416 A CN 105754416A CN 201610310793 A CN201610310793 A CN 201610310793A CN 105754416 A CN105754416 A CN 105754416A
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- China
- Prior art keywords
- preparation
- conductive ink
- electrically conductive
- solution
- zinc
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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
-
- 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
Abstract
The invention relates to the technical field of preparation of electronic technology materials, in particular to a preparation method of a conductive ink. The preparation method comprises the following steps: (1) preparation of a nanoparticle conductive material; (2) preparation of zinc oxide composite silver powder; (3) preparation of the conductive ink. The composite conductive ink provided by the invention has a low silver content and is low in preparation cost. Graphene/polyaniline composite conductive powder is selected, benefitted from the special lamellar structure of graphene, graphene can play a conductive connecting role, and meanwhile, conductive polyaniline also has high conductivity, so that the composite conductive powder prepared by doping of the two has high conductivity. According to the preparation method, the addition of silver powder is greatly reduced, and the prepared conductive ink also has excellent conductivity. The selected zinc oxide composite silver powder can improve the dispersion stability of traditional silver powder in the conductive ink.
Description
Technical field
The present invention relates to electronic technology technical field of material, the preparation method being specifically related to a kind of electrically conductive ink.
Background technology
Electrically conductive ink is a kind of conductive composite material being dispersed in link stuff by metallic conducting particle (silver, copper, carbon, be generally silver) to be formed, and after being printed onto on stock, plays the effect of wire, antenna and resistance.Electrically conductive ink be produce organic printed circuit board (thin film) the most basic, be also the raw material of most critical, its application in fields such as membrane switch panel, keyboard, compliant conductive winding displacement, electronic shield, RF identification is more and more extensive, is one of critical materials that decide organic print electronic product success or failure.
Existing electrically conductive ink is much made up of conductive noble metal microgranule, expensive, and other metal powders beyond desilver powder are easy to oxidation and reduce electric conductivity.Although and the electrically conductive ink of carbon dust is with low cost, but electric conductivity is poor, limit its application.
Therefore, the starting point of the present invention is in that how to prepare the electrically conductive ink that a kind of electric conductivity is excellent, stability is high, price is low.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of electrically conductive ink, the electric conductivity of this electrically conductive ink is excellent, stability is high, price is low.
Realizing the preparation method that the object of the invention be the technical scheme is that a kind of electrically conductive ink, it includes being made by step:
1) preparation of nanoparticle conductive material: graphene oxide is put into ultrasonic disperse in dehydrated alcohol, is subsequently adding aniline, under magnetic stirring mix homogeneously, prepares the first solution；Ammonium persulfate. is placed in high chloro acid solution, ultrasonic disperse, prepare the second solution；Second solution is slowly dropped in the first solution, at 0～40 DEG C, react 1～3h, finally successively sucking filtration, distilled water wash, vacuum drying, pulverizing；
2) preparation of zinc oxide silver powder: be impregnated in by argentum powder in zinc solution, stir, prepares mixed liquor；Prepared mixed liquor is evaporated, and is put in baking oven and is dried, be subsequently placed in Muffle furnace, carry out high-temperature roasting, namely prepare described zinc oxide silver powder；
3) preparation of electrically conductive ink: by step 1) prepare nanoparticle conductive material, step 2) prepare zinc oxide silver powder, binding agent and stirring solvent uniformly.
Wherein, step 1) described in the mass volume ratio of graphene oxide and dehydrated alcohol be 1g:10～100mL, the mass volume ratio of described graphene oxide and aniline is 1g:5～15mL, the mass volume ratio of described Ammonium persulfate. and aniline is 1～3g:1mL, and described high chloro acid solution's concentration is 0.5～1mol/L.
Step 2) described in the mass volume ratio of argentum powder and zinc solution be 1g:10～50mL, described zinc solution concentration is 0.1～1mol/L, and described zinc salt is zinc nitrate or zinc acetate.
Step 3) in parts by weight, described nanoparticle conductive material 5～85%, zinc oxide silver powder 1～83%, binding agent 2～6% and solvent 5～10%.
Preferably, step 2) described in high-temperature roasting, its roasting condition is: under excess oxygen, with the ramp of 5 DEG C/min to 350～380 DEG C, keeps 1～3 hour.
It is further preferred that step 2) described in the mean diameter of argentum powder be 1.3～2.0 μm.
It is furthermore preferred that step 3) described in binding agent one in epoxy resin, acrylic resin, polyurethane resin, organic siliconresin；Described solvent one in terpineol, Oleum Terebinthinae, butyl ether, butyl carbitol.
The technological merit of the present invention is as follows:
1) the graphene/polyaniline composite conductive powder that the present invention selects, has benefited from the lamellar structure that Graphene is special, has an effect of conductive communication, and electrically conductive polyaniline also has high conductivity simultaneously, and both have high conductivity at the prepared composite conductive powder that adulterates.The present invention greatly reduces the addition of argentum powder, and obtained electrically conductive ink has the electric conductivity of excellence equally.
2) the zinc oxide silver powder that the present invention selects can improve tradition argentum powder dispersion stabilization in electrically conductive ink.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) preparation of graphene/polyaniline composite conductive powder
3g graphene oxide is put into ultrasonic disperse in 30mL dehydrated alcohol, is subsequently adding 15mL aniline, under magnetic stirring mix homogeneously, prepare the first solution；15g Ammonium persulfate. is placed in 1mol/L high chloro acid solution, ultrasonic disperse, prepare the second solution；Second solution is slowly dropped in the first solution, at 20 DEG C, react 2h, finally successively sucking filtration, distilled water wash, vacuum drying, pulverizing, namely prepare graphene/polyaniline composite conductive powder.
2) preparation of zinc oxide silver powder
The argentum powder of 5g mean diameter 1.5 μm be impregnated in 100mL concentration is in 0.5mol/L zinc nitrate solution, stirs, and prepares mixed liquor；Prepared mixed liquor is evaporated, and is put in baking oven and is dried, be subsequently placed in Muffle furnace, carry out high-temperature roasting, its roasting condition is: under excess oxygen, with the ramp of 5 DEG C/min to 350 DEG C, keeps 2 hours namely preparing described zinc oxide silver powder.
3) preparation of electrically conductive ink
In parts by weight, by step 1) the nanoparticle conductive material 5% for preparing, step 2) the zinc oxide silver powder 83%, epoxy resin of binder 2% and solvent terpineol or the Oleum Terebinthinae 10% that prepare stir.
Embodiment 2
1) preparation of graphene/polyaniline composite conductive powder
3g graphene oxide is put into ultrasonic disperse in 100mL dehydrated alcohol, is subsequently adding 45mL aniline, under magnetic stirring mix homogeneously, prepare the first solution；135g Ammonium persulfate. is placed in 0.5mol/L high chloro acid solution, ultrasonic disperse, prepare the second solution；Second solution is slowly dropped in the first solution, at 40 DEG C, react 1h, finally successively sucking filtration, distilled water wash, vacuum drying, pulverizing, namely prepare graphene/polyaniline composite conductive powder.
2) preparation of zinc oxide silver powder
The argentum powder of 5g mean diameter 1.3 μm be impregnated in 250mL concentration is in 1mol/L zinc acetate solution, stirs, and prepares mixed liquor；Prepared mixed liquor is evaporated, and is put in baking oven and is dried, be subsequently placed in Muffle furnace, carry out high-temperature roasting, its roasting condition is: under excess oxygen, with the ramp of 5 DEG C/min to 380 DEG C, keeps 3 hours namely preparing described zinc oxide silver powder.
3) preparation of electrically conductive ink
In parts by weight, by step 1) the nanoparticle conductive material 85% for preparing, step 2) the zinc oxide silver powder 1% for preparing, binding agent polyurethane resin 6% and solvent butyl ether 8% stir.
Embodiment 3
1) preparation of graphene/polyaniline composite conductive powder
3g graphene oxide is put into ultrasonic disperse in 50mL dehydrated alcohol, is subsequently adding 30mL aniline, under magnetic stirring mix homogeneously, prepare the first solution；60g Ammonium persulfate. is placed in 0.5mol/L high chloro acid solution, ultrasonic disperse, prepare the second solution；Second solution is slowly dropped in the first solution, at 0 DEG C, react 3h, finally successively sucking filtration, distilled water wash, vacuum drying, pulverizing, namely prepare graphene/polyaniline composite conductive powder.
2) preparation of zinc oxide silver powder
The argentum powder of 5g mean diameter 2.0 μm be impregnated in 150mL concentration is in 0.1mol/L zinc nitrate solution, stirs, and prepares mixed liquor；Prepared mixed liquor is evaporated, and is put in baking oven and is dried, be subsequently placed in Muffle furnace, carry out high-temperature roasting, its roasting condition is: under excess oxygen, with the ramp of 5 DEG C/min to 350 DEG C, keeps 1 hour namely preparing described zinc oxide silver powder.
3) preparation of electrically conductive ink
In parts by weight, by step 1) the nanoparticle conductive material 60% for preparing, step 2) the zinc oxide silver powder 30% for preparing, binding agent organic siliconresin 5% and solvent butyl carbitol 5% stir.
Claims (8)
1. the preparation method of an electrically conductive ink, it is characterised in that: include being made by step:
1) preparation of nanoparticle conductive material: graphene oxide is put into ultrasonic disperse in dehydrated alcohol, is subsequently adding aniline, under magnetic stirring mix homogeneously, prepares the first solution；Ammonium persulfate. is placed in high chloro acid solution, ultrasonic disperse, prepare the second solution；Second solution is slowly dropped in the first solution, at 0～40 DEG C, react 1～3h, finally successively sucking filtration, distilled water wash, vacuum drying, pulverizing；
2) preparation of zinc oxide silver powder: be impregnated in by argentum powder in zinc solution, stir, prepares mixed liquor；Prepared mixed liquor is evaporated, and is put in baking oven and is dried, be subsequently placed in Muffle furnace, carry out high-temperature roasting, namely prepare described zinc oxide silver powder；
3) preparation of electrically conductive ink: by step 1) prepare nanoparticle conductive material, step 2) prepare zinc oxide silver powder, binding agent and stirring solvent uniformly.
2. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterized in that: step 1) described in the mass volume ratio of graphene oxide and dehydrated alcohol be 1g:10～100mL, the mass volume ratio of described graphene oxide and aniline is 1g:5～15mL, the mass volume ratio of described Ammonium persulfate. and aniline is 1～3g:1mL, and described high chloro acid solution's concentration is 0.5～1mol/L.
3. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterized in that: step 2) described in the mass volume ratio of argentum powder and zinc solution be 1g:10～50mL, described zinc solution concentration is 0.1～1mol/L, and described zinc salt is zinc nitrate or zinc acetate.
4. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterized in that: step 3) in parts by weight, described nanoparticle conductive material 5～85%, zinc oxide silver powder 1～83%, binding agent 2～6% and solvent 5～10%.
5. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterised in that: step 2) described in high-temperature roasting, its roasting condition is: under excess oxygen, with the ramp of 5 DEG C/min to 350～380 DEG C, keeps 1～3 hour.
6. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterised in that: step 2) described in the mean diameter of argentum powder be 1.3～2.0 μm.
7. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterised in that: step 3) described in binding agent one in epoxy resin, acrylic resin, polyurethane resin, the organic siliconresin.
8. the preparation method of a kind of electrically conductive ink according to claim 1, it is characterised in that: step 3) described in solvent one in terpineol, Oleum Terebinthinae, butyl ether, the butyl carbitol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610310793.6A CN105754416A (en) | 2016-05-12 | 2016-05-12 | Preparation method of conductive ink |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610310793.6A CN105754416A (en) | 2016-05-12 | 2016-05-12 | Preparation method of conductive ink |
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| CN105754416A true CN105754416A (en) | 2016-07-13 |
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| CN201610310793.6A Pending CN105754416A (en) | 2016-05-12 | 2016-05-12 | Preparation method of conductive ink |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108753045A (en) * | 2018-06-11 | 2018-11-06 | 江苏海田电子材料有限公司 | A kind of electrically conductive ink |
| CN110172293A (en) * | 2019-04-29 | 2019-08-27 | 中南大学 | A kind of UV solidification transparent conductive coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101137730A (en) * | 2005-03-11 | 2008-03-05 | 东洋油墨制造株式会社 | Electrically conductive ink, electrically conductive circuit, and noncontact-type medium |
| CN103319954A (en) * | 2013-07-12 | 2013-09-25 | 珠海市乐通化工股份有限公司 | Conductive graphene printing ink and preparation method thereof |
| CN104031433A (en) * | 2014-06-09 | 2014-09-10 | 大连理工大学 | Low-conductivity flake graphene composite material, and preparation method and application thereof |
-
2016
- 2016-05-12 CN CN201610310793.6A patent/CN105754416A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101137730A (en) * | 2005-03-11 | 2008-03-05 | 东洋油墨制造株式会社 | Electrically conductive ink, electrically conductive circuit, and noncontact-type medium |
| CN103319954A (en) * | 2013-07-12 | 2013-09-25 | 珠海市乐通化工股份有限公司 | Conductive graphene printing ink and preparation method thereof |
| CN104031433A (en) * | 2014-06-09 | 2014-09-10 | 大连理工大学 | Low-conductivity flake graphene composite material, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 庹度: ""载银氧化锌复合纳米粒子的制备与表征"", 《包装学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108753045A (en) * | 2018-06-11 | 2018-11-06 | 江苏海田电子材料有限公司 | A kind of electrically conductive ink |
| CN110172293A (en) * | 2019-04-29 | 2019-08-27 | 中南大学 | A kind of UV solidification transparent conductive coating and preparation method thereof |
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Application publication date: 20160713 |