CN108659624A - A kind of preparation method of nano silver composite conducting ink - Google Patents
A kind of preparation method of nano silver composite conducting ink Download PDFInfo
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- CN108659624A CN108659624A CN201810341994.1A CN201810341994A CN108659624A CN 108659624 A CN108659624 A CN 108659624A CN 201810341994 A CN201810341994 A CN 201810341994A CN 108659624 A CN108659624 A CN 108659624A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/103—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds of aldehydes, e.g. phenol-formaldehyde resins
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a kind of preparation methods of nano silver composite conducting ink; it is first that silver-colored forerunner, ascorbic acid and citric acid make reducing agent, polyvinylpyrrolidone as protective agent using silver nitrate; the nano silver colloid of size tunable, good dispersion, soilless sticking phenomenon is made using liquid phase reduction; then aqueous acrylic urethane resins, amino resins, polyvinyl alcohol, nano silver powder, graphene, antifoaming agent, dispersant, sodium carboxymethylcellulose, water are mixed; dispersion to get.Gained electrically conductive ink not only has higher electric conductivity, but also has good cohesive force.
Description
Technical field
The invention belongs to printed electronic field of material technology, and in particular to a kind of preparation side of nano silver composite conducting ink
Method.
Background technology
The continuous Transformation Development of printing industry permeates with the blendings of other industries in addition, the emerging printed electronic skill of growth-promoting
Art.It is photovoltaic cell, wireless radio frequency identification mark, thin currently, using most functional materials be electrically conductive ink in printed electronic
Membrane switch etc. is all electrically conductive ink industrialization production and widely applied mark.However, not along with printing and electronic industry
Disconnected development, the requirement to electrically conductive ink product are continuously improved, and the connected applications of nanotechnology and electrically conductive ink have been increasingly becoming one
The new development trend of kind.
Electrically conductive ink refers to the fully dispersed substance obtained in a solvent with conducting function of conducting particles and binder.
Silver is material most potential in electrically conductive ink, and research at present is most due to having good conductive property and physicochemical property
More materials.As nanotechnology is constantly progressive, and good nature possessed by silver itself, nano silver is widely used in various
Field, such as analysis detection, electrically conductive ink, biological study, medical research, catalyticing research, optical research etc..Nano silver conductive ink
With its excellent conductivity, good chemical stability, moderate price, preparation process is convenient, is not necessarily to additional anti-oxidation measure
The advantages that, become the focus in electrically conductive ink research hotspot.But nano silver particles that there is also grain sizes is difficult to control simultaneously, point
The defects of property is poor, electric conductivity is easily affected by temperature is dissipated, therefore, green, prepared by quick, size tunable nano silver, it is in oil
It is that current nanometer silver ink needs solve that fine dispersion and water-based ink in ink, which prepare and be adapted to various printable fabrics,
Critical issue.
Invention content
The object of the present invention is to provide a kind of preparation methods of nano silver composite conducting ink.
A kind of preparation method of nano silver composite conducting ink, includes the following steps：
Step 1, in parts by weight, by silver nitrate 0.5-1 parts add in 5-10 parts of water, stir evenly, add dispersant 0.1-
0.2 part and 0.1-0.2 parts of protective agent, stirring adjust pH of mixed to 7-8, and insulated and stirred under the conditions of 60 DEG C is dripped while stirring
Add 0.05-0.1 parts of reducing agent solution, continues to be stirred to react 1h, obtain nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 20-30 parts of aqueous acrylic urethane resins, 2-4 parts of amino resins, polyvinyl alcohol 1-5
Part, 20-30 parts of nano silver powder, 2-5 parts of graphene, 1-3 parts of antifoaming agent, 1-4 parts of dispersant, 1-3 parts of sodium carboxymethylcellulose,
The mixing of 100 parts of water, dispersion to get.
Preferably, dispersant described in step 1 is calgon.
Preferably, the protective agent is polyvinylpyrrolidone.
Preferably, also added with gelatin in the protective agent, addition is the 1/10 of polyvinylpyrrolidone dosage.
Preferably, the reducing agent solution is the mixed liquor of ascorbic acid and citric acid.
Preferably, dispersant described in step 3 is polyethylene glycol 400.
The present invention is that silver-colored forerunner, ascorbic acid and citric acid make reducing agent, polyvinylpyrrolidone as protection using silver nitrate
The nano silver colloid of size tunable, good dispersion, soilless sticking phenomenon is made using liquid phase reduction for agent.Select water soluble acrylic acid
Polyurethane resin, amino resins and polyvinyl alcohol it is compound be used as link stuff, that is, overcome the defect of acrylic resin coloring difference,
Again with high intensity, tear-proof, wear-resisting advantage.
Specific implementation mode
Embodiment 1
A kind of preparation method of nano silver composite conducting ink, includes the following steps：
Step 1, in parts by weight, by silver nitrate 0.5 part add in 5 parts of water, stir evenly, add 0.1 part of dispersant and protect
0.1 part of agent is protected, stirring adjusts pH of mixed to 7-8, and reducing agent solution is added dropwise in insulated and stirred under the conditions of 60 DEG C while stirring
0.05 part, continues to be stirred to react 1h, obtain nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 20 parts of aqueous acrylic urethane resins, 2 parts of amino resins, polyvinyl alcohol 1 part, nanometer
100 parts of 20 parts of aluminium powder, 2 parts of graphene, 1 part of antifoaming agent, 1 part of dispersant, 1 part of sodium carboxymethylcellulose, water mixing, dispersion,
To obtain the final product.
Wherein, dispersant described in step 1 is calgon.The protective agent is polyvinylpyrrolidone.It is described to go back
Former agent solution is the mixed liquor of ascorbic acid and citric acid, and the total concentration of ascorbic acid and citric acid is 20wt.%, ascorbic acid
Concentration ratio with citric acid is 2：1.Dispersant described in step 3 is polyethylene glycol 400.
In addition, also added with gelatin in protective agent, addition is the 1/10 of polyvinylpyrrolidone dosage.
Gained electrically conductive ink is used into flexographic printing techniques, is printed on PP plates, then is done under conditions of temperature is 100 DEG C
Dry solidification 4h, it is 10 μm of conductive oil ink film to finally obtain thickness, is detected to conductive oil ink film, resistivity is 6.2 ×
10-4Ω·cm；Hardness test is carried out to it using Chinese pencil according to national standard GB/T 6739-1996, using Chinese pencil to it
Carry out hardness test, hardness 3H；According to national standard GB/T 13217.4-2008, adhesive force is tested using 3M special adhesive tapes,
Adhesive force 100%.
Embodiment 2
A kind of preparation method of nano silver composite conducting ink, includes the following steps：
Step 1, in parts by weight, by silver nitrate 0.7 part add in 6 parts of water, stir evenly, add 0.1 part of dispersant and protect
0.2 part of agent is protected, stirring adjusts pH of mixed to 7-8, and reducing agent solution is added dropwise in insulated and stirred under the conditions of 60 DEG C while stirring
0.07 part, continues to be stirred to react 1h, obtain nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 23 parts of aqueous acrylic urethane resins, 3 parts of amino resins, polyvinyl alcohol 3 part, nanometer
100 parts of 24 parts of aluminium powder, 3 parts of graphene, 2 parts of antifoaming agent, 2 parts of dispersant, 1 part of sodium carboxymethylcellulose, water mixing, dispersion,
To obtain the final product.
Wherein, dispersant described in step 1 is calgon.The protective agent is polyvinylpyrrolidone.It is described to go back
Former agent solution is the mixed liquor of ascorbic acid and citric acid, and the total concentration of ascorbic acid and citric acid is 20wt.%, ascorbic acid
Concentration ratio with citric acid is 2：1.Dispersant described in step 3 is polyethylene glycol 400.
In addition, also added with gelatin in protective agent, addition is the 1/10 of polyvinylpyrrolidone dosage.
Gained electrically conductive ink is used into flexographic printing techniques, is printed on PP plates, then is done under conditions of temperature is 100 DEG C
Dry solidification 4h, it is 10 μm of conductive oil ink film to finally obtain thickness, is detected to conductive oil ink film, resistivity is 6.5 ×
10-4Ω·cm；Hardness test is carried out to it using Chinese pencil according to national standard GB/T 6739-1996, using Chinese pencil to it
Carry out hardness test, hardness 3H；According to national standard GB/T 13217.4-2008, adhesive force is tested using 3M special adhesive tapes,
Adhesive force 100%.
Embodiment 3
A kind of preparation method of nano silver composite conducting ink, includes the following steps：
Step 1, in parts by weight, by silver nitrate 0.8 part add in 7 parts of water, stir evenly, add 0.2 part of dispersant and protect
0.1 part of agent is protected, stirring adjusts pH of mixed to 7-8, and reducing agent solution is added dropwise in insulated and stirred under the conditions of 60 DEG C while stirring
0.08 part, continues to be stirred to react 1h, obtain nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 27 parts of aqueous acrylic urethane resins, 3 parts of amino resins, polyvinyl alcohol 4 part, nanometer
100 parts of 27 parts of aluminium powder, 4 parts of graphene, 2 parts of antifoaming agent, 3 parts of dispersant, 2 parts of sodium carboxymethylcellulose, water mixing, dispersion,
To obtain the final product.
Wherein, dispersant described in step 1 is calgon.The protective agent is polyvinylpyrrolidone.It is described to go back
Former agent solution is the mixed liquor of ascorbic acid and citric acid, and the total concentration of ascorbic acid and citric acid is 20wt.%, ascorbic acid
Concentration ratio with citric acid is 2：1.Dispersant described in step 3 is polyethylene glycol 400.
In addition, also added with gelatin in protective agent, addition is the 1/10 of polyvinylpyrrolidone dosage.
Gained electrically conductive ink is used into flexographic printing techniques, is printed on PP plates, then is done under conditions of temperature is 100 DEG C
Dry solidification 4h, it is 10 μm of conductive oil ink film to finally obtain thickness, is detected to conductive oil ink film, resistivity is 7.2 ×
10-4Ω·cm；Hardness test is carried out to it using Chinese pencil according to national standard GB/T 6739-1996, using Chinese pencil to it
Carry out hardness test, hardness 3H；According to national standard GB/T 13217.4-2008, adhesive force is tested using 3M special adhesive tapes,
Adhesive force 100%.
Embodiment 4
A kind of preparation method of nano silver composite conducting ink, includes the following steps：
Step 1, in parts by weight, by silver nitrate 1 part add in 10 parts of water, stir evenly, add 0.2 part of dispersant and protection
0.2 part of agent, stirring adjust pH of mixed to 7-8, and reducing agent solution 0.1 is added dropwise in insulated and stirred under the conditions of 60 DEG C while stirring
Part, continue to be stirred to react 1h, obtains nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 30 parts of aqueous acrylic urethane resins, 4 parts of amino resins, polyvinyl alcohol 5 part, nanometer
100 parts of 30 parts of aluminium powder, 5 parts of graphene, 3 parts of antifoaming agent, 4 parts of dispersant, 3 parts of sodium carboxymethylcellulose, water mixing, dispersion,
To obtain the final product.
Wherein, dispersant described in step 1 is calgon.The protective agent is polyvinylpyrrolidone.It is described to go back
Former agent solution is the mixed liquor of ascorbic acid and citric acid, and the total concentration of ascorbic acid and citric acid is 20wt.%, ascorbic acid
Concentration ratio with citric acid is 2：1.Dispersant described in step 3 is polyethylene glycol 400.
In addition, also added with gelatin in protective agent, addition is the 1/10 of polyvinylpyrrolidone dosage.
Gained electrically conductive ink is used into flexographic printing techniques, is printed on PP plates, then is done under conditions of temperature is 100 DEG C
Dry solidification 4h, it is 10 μm of conductive oil ink film to finally obtain thickness, is detected to conductive oil ink film, resistivity is 6.1 ×
10-4Ω·cm；Hardness test is carried out to it using Chinese pencil according to national standard GB/T 6739-1996, using Chinese pencil to it
Carry out hardness test, hardness 3H；According to national standard GB/T 13217.4-2008, adhesive force is tested using 3M special adhesive tapes,
Adhesive force 100%.
Claims (6)
1. a kind of preparation method of nano silver composite conducting ink, it is characterised in that：Include the following steps：
Step 1, in parts by weight, by silver nitrate 0.5-1 parts add in 5-10 parts of water, stir evenly, add dispersant 0.1-
0.2 part and 0.1-0.2 parts of protective agent, stirring adjust pH of mixed to 7-8, and insulated and stirred under the conditions of 60 DEG C is dripped while stirring
Add 0.05-0.1 parts of reducing agent solution, continues to be stirred to react 1h, obtain nano-silver colloid；
Step 2, nano-silver colloid is centrifuged, EtOH Sonicate dispersion is added after outwelling supernatant, outwells supernatant after centrifuging again, weight
After backwashing is washed 3 times, dry, obtains nano silver powder；
Step 3, in parts by weight, by 20-30 parts of aqueous acrylic urethane resins, 2-4 parts of amino resins, polyvinyl alcohol 1-5
Part, 20-30 parts of nano silver powder, 2-5 parts of graphene, 1-3 parts of antifoaming agent, 1-4 parts of dispersant, 1-3 parts of sodium carboxymethylcellulose,
The mixing of 100 parts of water, dispersion to get.
2. the preparation method of nano silver composite conducting ink according to claim 1, it is characterised in that：Described in step 1
Dispersant is calgon.
3. the preparation method of nano silver composite conducting ink according to claim 1, it is characterised in that：The protective agent is
Polyvinylpyrrolidone.
4. the preparation method of nano silver composite conducting ink according to claim 3, it is characterised in that：In the protective agent
Also added with gelatin, addition is the 1/10 of polyvinylpyrrolidone dosage.
5. the preparation method of nano silver composite conducting ink according to claim 1, it is characterised in that：The reducing agent is molten
Liquid is the mixed liquor of ascorbic acid and citric acid.
6. the preparation method of nano silver composite conducting ink according to claim 1, it is characterised in that：Described in step 3
Dispersant is polyethylene glycol 400.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN110776786A (en) * | 2019-12-18 | 2020-02-11 | 武汉华知智能科技有限公司 | Graphene nano-silver composite conductive ink and preparation method thereof |
| CN110862503A (en) * | 2019-11-29 | 2020-03-06 | 佛山市瑞福物联科技有限公司 | Preparation method of conductive polyurethane prepolymer and conductive adhesive thereof |
| CN111253845A (en) * | 2020-03-09 | 2020-06-09 | 广东四维新材料有限公司 | Nano-silver antibacterial spray-formed protective film and preparation method thereof |
| CN111560188A (en) * | 2020-06-01 | 2020-08-21 | 南京林业大学 | Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof |
| CN112059205A (en) * | 2020-09-18 | 2020-12-11 | 东北大学 | Preparation method of nano-silver with stable particle size |
| CN112625508A (en) * | 2021-01-12 | 2021-04-09 | 陕西科技大学 | Preparation method of graphene conductive ink for 3D printing on paper |
Citations (3)
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|---|---|---|---|---|
| CN104263082A (en) * | 2014-08-29 | 2015-01-07 | 南京航空航天大学 | Graphene organic silver conductive printing ink and preparation method thereof |
| CN104923801A (en) * | 2014-03-17 | 2015-09-23 | 北京中科纳通电子技术有限公司 | Method for preparing nanosilver powder in batches |
| CN107793842A (en) * | 2017-10-20 | 2018-03-13 | 西安理工大学 | A kind of preparation method of Nano silver conductive ink |
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| CN104923801A (en) * | 2014-03-17 | 2015-09-23 | 北京中科纳通电子技术有限公司 | Method for preparing nanosilver powder in batches |
| CN104263082A (en) * | 2014-08-29 | 2015-01-07 | 南京航空航天大学 | Graphene organic silver conductive printing ink and preparation method thereof |
| CN107793842A (en) * | 2017-10-20 | 2018-03-13 | 西安理工大学 | A kind of preparation method of Nano silver conductive ink |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN109535847B (en) * | 2018-11-26 | 2021-12-28 | 国宏中晶集团有限公司 | Graphene-containing conductive ink, preparation method thereof and flexible paper-based conductive circuit |
| CN110862503A (en) * | 2019-11-29 | 2020-03-06 | 佛山市瑞福物联科技有限公司 | Preparation method of conductive polyurethane prepolymer and conductive adhesive thereof |
| CN110862503B (en) * | 2019-11-29 | 2022-02-11 | 佛山市瑞福物联科技有限公司 | Preparation method of conductive polyurethane prepolymer and conductive adhesive thereof |
| CN110776786A (en) * | 2019-12-18 | 2020-02-11 | 武汉华知智能科技有限公司 | Graphene nano-silver composite conductive ink and preparation method thereof |
| CN111253845A (en) * | 2020-03-09 | 2020-06-09 | 广东四维新材料有限公司 | Nano-silver antibacterial spray-formed protective film and preparation method thereof |
| CN111560188A (en) * | 2020-06-01 | 2020-08-21 | 南京林业大学 | Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof |
| CN112059205A (en) * | 2020-09-18 | 2020-12-11 | 东北大学 | Preparation method of nano-silver with stable particle size |
| CN112625508A (en) * | 2021-01-12 | 2021-04-09 | 陕西科技大学 | Preparation method of graphene conductive ink for 3D printing on paper |
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Application publication date: 20181016 |