CN101979708B - Method for preparing carbon nano tube silvered acrylic acid series electromagnetic shielding coating - Google Patents
Method for preparing carbon nano tube silvered acrylic acid series electromagnetic shielding coating Download PDFInfo
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- CN101979708B CN101979708B CN2010105058161A CN201010505816A CN101979708B CN 101979708 B CN101979708 B CN 101979708B CN 2010105058161 A CN2010105058161 A CN 2010105058161A CN 201010505816 A CN201010505816 A CN 201010505816A CN 101979708 B CN101979708 B CN 101979708B
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Abstract
The invention discloses a method for preparing a carbon nano tube silvered acrylic acid series electromagnetic shielding coating. The method comprises the following steps of: plating a layer of nickel on the surface of CNTs (carbon nano tubes) by adopting a chemical plating method, and then performing chemical silvering to obtain a silvered CNTs composite filler which takes the CNTs with high length-diameter ratio as cores and takes a uniform silvering layer as a shell; and mixing the prepared silvered CNTs, acrylic resin, ethyl acetate and n-butyl alcohol in a ratio, and dispersing the mixture uniformly to finally prepare the electromagnetic shielding coating with good electric conductivity and electromagnetic shielding effect. The layer of nickel is uniformly plated on the surface of the CNTs before the chemical silvering so that the bonding force between the silvering layer and the CNTs is improved and the silvered CNTs have better electric conductivity and dispersibility and are favorable for application in the electromagnetic shielding material field.
Description
Technical field
The present invention relates to the preparation method of the silver-plated acrylic acid series electromagnetic screen coating of a kind of carbon nanotube, prepared silver-plated carbon nanotube can be applicable to the electromagnetic shielding composite material field.
Background technology
The developing trend of hyundai electronics circuit and element is in microminiaturized, integrated, lightweight and digitizing; And these electronic products adopt light weight, specious plastics to make shell more; But these plastics have no protective capacities to hertzian wave; So regular meeting makes electronic product receive the interference (being EMI) of external electromagnetic ripple and malfunction, image obstacle and voice disorder etc. occur, thereby has formed the problem of hertzian wave public hazards.For solving the electromagnetic interference (EMI) problem, electromagnetic shielding material is developed rapidly.In various electromagnetic shielding materials, electromagnetic screen coating is with a wide range of applications as a kind of efficient, cheap, light weight, convenient application technique means.
Using at present more is composite electromagnetic shielding coating, and it is to be filmogen with the insulation superpolymer, is conductive medium with the filler grain with better conductivity, is applied to behind the mixed grinding on the workpiece, at a certain temperature film-forming.Acrylic coating all has special advantages at aspects such as weathering resistance, stain resistance, acidproof, alkaline-resisting, mechanical property, oil resistant and solvent resistances, is favored widely in industry and covil construction field, can be used as the filmogen of electrically conducting coating.Carbon nanotube (CNTs) has great length-to-diameter ratio and excellent electricity, magnetic performance, showing excellent performance aspect conduction and the shielding of suction ripple, so its research and development as the conductive filler material of electromagnetic screen coating comes into one's own more and more.But it is difficult for disperseing, and contact resistance is bigger, and its practical application is restricted.Plate one deck silver on the CNTs surface, both can improve dispersiveness, the electroconductibility of filler, keep the characteristics of CNTs big L/D ratio again, can reduce amount of filler and cost.
Summary of the invention
First purpose of the present invention provides the preparation method of the silver-plated acrylic acid series electromagnetic screen coating of a kind of carbon nanotube.
It is complex conductive fillers--silver-plated CNTs and preparation method thereof that kernel, its external parcel have the metallic silver layer of good electric conductivity with the CNTs with big L/D ratio that second purpose of the present invention provides a kind of.
Technical scheme of the present invention is following:
(1) 2.0g CNTs is added in an amount of 63% the concentrated nitric acid, the about 4h of ultra-sonic oscillation, filter the back with deionized water wash to neutral, the tin protochloride (SnCl that is preparing in advance respectively then
2) sensitizing solution and Palladous chloride (PdCl
2) carry out sensitization and activation 5～20min in the activation solution, sensitization and reactivation process are all disperseed with UW, filter then, and washing is to neutral;
(2) CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 2～20ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 10～20min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid begins the chemical nickel plating reaction, and the reaction times is 30min, filters at last, washes three times;
(3) nickel plating CNTs and deionized water are made into the 100ml suspension liquid; Add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt; Ultra-sonic dispersion 2min slowly drips the 100ml silver ammino solution then, puts into 70 ℃ of air dry ovens after the filtration washing and dries;
(4) getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1～2h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.
The described SnCl of step (1)
2Sensitizing solution and PdCl
2Activation solution, SnCl
2Consisting of of sensitizing solution: SnCl
20.1mol/L, HCl10ml/L; PdCl
2Consisting of of activation solution: PdCl
20.0014mol/L, HCl 25ml/L.
The said hyperacoustic power of step (1) is 800W.
The composition of the described complexed surfactant of step (2) is: X 2073 (SDBS) and OP-10, both mass ratioes are 2: 1.
Consisting of of step (2) described chemical nickel plating reaction solution: NiSO
430g/L, Trisodium Citrate 10～90g/L, trolamine 10～90ml/L, NaH
2PO
210～30g/L.
Consisting of of step (3) described silver ammino solution: AgNO
350～150g/L, ammoniacal liquor 250ml/L.
Step (4) is described evenly to be coated it on kraft paper substrate with line rod spreader, and its coating thickness is 200 μ m.
Beneficial effect of the present invention:
The method of general at present use electroless plating directly plates one deck silver (single stage method) on the CNTs surface.The present invention has obtained the good silver-plated CNTs of electroconductibility through CNTs being carried out chemical nickel plating silver-plated again (two-step approach) earlier, with the acrylic acid series electromagnetic screen coating of making conductive filler material have good electrical conductivity and effectiveness.
Embodiment
Through specific examples the present invention is further described.
Embodiment 1:
2.0g CNTs is added in the concentrated nitric acid of 150ml 63%, the about 4h of ultra-sonic oscillation, extremely neutral after filtering with deionized water wash.The SnCl that is preparing in advance respectively then
2Sensitizing solution and PdCl
2Carry out sensitization and activation 10min in the activation solution, sensitization and reactivation process are all disperseed with the UW of 800W power.Filter then, washing is to neutral.CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 2ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 20min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid begins the chemical nickel plating reaction, and the chemical nickel plating reaction solution consists of: NiSO
430g/L, Trisodium Citrate 10g/L, trolamine 90ml/L, NaH
2PO
230g/L.Reaction times is 30min.Filter at last, wash three times.Nickel plating CNTs and deionized water are made into the 100ml suspension liquid, add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt, 800W ultra-sonic dispersion 2min slowly drips 100ml AgNO then
3Concentration is the silver ammino solution of 100g/L.Putting into 70 ℃ of air dry ovens after the filtration washing dries.Getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 2h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.The volume specific resistance of prepared composite electromagnetic screen coating is 14.8m Ω cm, and the electromagnet shield effect in 3.95～5.85GHz range of frequency is 20.5～26dB.
Embodiment 2:
2.0g CNTs is added in the concentrated nitric acid of 150ml 63%, the about 4h of ultra-sonic oscillation, extremely neutral after filtering with deionized water wash.The SnCl that is preparing in advance respectively then
2Sensitizing solution and PdCl
2Carry out sensitization and activation 5min in the activation solution, sensitization and reactivation process are all disperseed with the UW of 800W power.Filter then, washing is to neutral.CNTs after the activation and deionized water are made into the 200ml suspension liquid, and adding 10ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 10min; Add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 50g Seignette salt, 800W ultra-sonic dispersion 2min then; The last 100ml AgNO that slowly drips
3Concentration is the silver ammino solution of 100g/L.Putting into 70 ℃ of air dry ovens after the filtration washing dries.Getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.The volume specific resistance of prepared composite electromagnetic screen coating is 52.9m Ω cm, and the electromagnet shield effect in 3.95～5.85GHz range of frequency is 13～16.7dB.
Embodiment 3:
2.0g CNTs is added in the concentrated nitric acid of 150ml 63%, the about 4h of ultra-sonic oscillation, extremely neutral after filtering with deionized water wash.The SnCl that is preparing in advance respectively then
2Sensitizing solution and PdCl
2Carry out sensitization and activation 20min in the activation solution, sensitization and reactivation process are all disperseed with the UW of 800W power.Filter then, washing is to neutral.CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 20ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 15min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid begins the chemical nickel plating reaction, and the chemical nickel plating reaction solution consists of: NiSO
430g/L, Trisodium Citrate 10g/L, trolamine 70ml/L, NaH
2PO
220g/L.Reaction times is 30min.Filter at last, wash three times.Nickel plating CNTs and deionized water are made into the 100ml suspension liquid, add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt, 800W ultra-sonic dispersion 2min slowly drips 100ml AgNO then
3Concentration is the silver ammino solution of 100g/L.Putting into 70 ℃ of air dry ovens after the filtration washing dries.Getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.The volume specific resistance of prepared composite electromagnetic screen coating is 10.5m Ω cm, and the electromagnet shield effect in 3.95～5.85GHz range of frequency is 24～29.5dB.
Embodiment 4:
2.0g CNTs is added in the concentrated nitric acid of 150ml 63%, the about 4h of ultra-sonic oscillation, extremely neutral after filtering with deionized water wash.The SnCl that is preparing in advance respectively then
2Sensitizing solution and PdCl
2Carry out sensitization and activation 10min in the activation solution, sensitization and reactivation process are all disperseed with the UW of 800W power.Filter then, washing is to neutral.CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 20ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 20min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid begins the chemical nickel plating reaction, and the chemical nickel plating reaction solution consists of: NiSO
430g/L, Trisodium Citrate 90g/L, trolamine 10ml/L, NaH
2PO
210g/L.Reaction times is 30min.Filter at last, wash three times.Nickel plating CNTs and deionized water are made into the 100ml suspension liquid, add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt, 800W ultra-sonic dispersion 2min slowly drips 100ml AgNO then
3Concentration is the silver ammino solution of 100g/L.Putting into 70 ℃ of air dry ovens after the filtration washing dries.Getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.The volume specific resistance of prepared composite electromagnetic screen coating is 16.0m Ω cm, and the electromagnet shield effect in 3.95～5.85GHz range of frequency is 19.5～24dB.
Embodiment 5:
2.0g CNTs is added in the concentrated nitric acid of 150ml 63%, the about 4h of ultra-sonic oscillation, extremely neutral after filtering with deionized water wash.The SnCl that is preparing in advance respectively then
2Sensitizing solution and PdCl
2Carry out sensitization and activation 15min in the activation solution, sensitization and reactivation process are all disperseed with the UW of 800W power.Filter then, washing is to neutral.CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 20ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2PO
2, stir 20min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid begins the chemical nickel plating reaction, and the chemical nickel plating reaction solution consists of: NiSO
430g/L, Trisodium Citrate 50g/L, trolamine 90ml/L, NaH
2PO
220g/L.Reaction times is 30min.Filter at last, wash three times.Nickel plating CNTs and deionized water are made into the 100ml suspension liquid, add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt, 800W ultra-sonic dispersion 2min slowly drips 100ml AgNO then
3Concentration is the silver ammino solution of 100g/L.Putting into 70 ℃ of air dry ovens after the filtration washing dries.Getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1.5h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.The volume specific resistance of prepared composite electromagnetic screen coating is 1.1m Ω cm, and the electromagnet shield effect in 3.95～5.85GHz range of frequency is 46.5～53dB.
Claims (7)
1. the preparation method of the silver-plated acrylic acid series electromagnetic screen coating of carbon nanotube is characterized in that this method may further comprise the steps:
(1) 2.0g CNTs is added in an amount of 63% the concentrated nitric acid, ultra-sonic oscillation 4h, filter the back with deionized water wash to neutral, the tin protochloride (SnCl that is preparing in advance respectively then
2) sensitizing solution and Palladous chloride (PdCl
2) carry out sensitization and activation 5～20min in the activation solution, sensitization and reactivation process are all disperseed with UW, filter then, and washing is to neutral;
(2) CNTs after the activation and deionized water are made into the 150ml suspension liquid, and adding 2～20ml mass concentration is 3% complexed surfactant solution, stirs, and adds 0.05g NaH behind the ultrasonic dispersing 1min
2P0
2, stir 10～20min; Slowly add the NiSO for preparing then
4Complex liquid and NaH
2PO
2Reduced liquid is that the chemical nickel plating reaction solution begins the chemical nickel plating reaction, and the reaction times is 30min, filters at last, washes three times;
(3) nickel plating CNTs and deionized water are made into the 100ml suspension liquid; Add the mixed solution 200ml that contains 15ml ethanol, 2ml complexed surfactant and 40g Seignette salt; Ultra-sonic dispersion 2min slowly drips the 100ml silver ammino solution then, puts into 70 ℃ of air dry ovens after the filtration washing and dries;
(4) getting 2.5g, to be scattered in the 17.5ml volume ratio through the silver-plated CNTs that grinds be in 6: 1 the ETHYLE ACETATE and n-butanol mixed solvent; Slowly add 2.5g acrylic solid resin; Magnetic rotation is stirred 1～2h and is made electromagnetic screen coating; With line rod spreader it is evenly coated on the kraft paper substrate then, dry naturally.
2. preparation method according to claim 1 is characterized in that: the described SnCl of step (1)
2Sensitizing solution and PdCl
2Activation solution, SnCl
2Consisting of of sensitizing solution: SnCl
20.1mol/L, HCl 10ml/L; PdCl
2Consisting of of activation solution: PdCl
20.0014mol/L, HCl 25ml/L.
3. preparation method according to claim 1 is characterized in that: the said hyperacoustic power of step (1) is 800W.
4. preparation method according to claim 1 is characterized in that: the composition of the described complexed surfactant of step (2) is: X 2073 (SDBS) and OP-10, both mass ratioes are 2: 1.
5. preparation method according to claim 1 is characterized in that: the consisting of of step (2) described chemical nickel plating reaction solution: NiSO
430g/L, Trisodium Citrate 10～90g/L, trolamine 10～90ml/L, NaH
2PO
210～30g/L.
6. preparation method according to claim 1 is characterized in that: the consisting of of step (3) described silver ammino solution: AgNO
3350～150g/L, ammoniacal liquor 250ml/L.
7. preparation method according to claim 1 is characterized in that: step (4) is described evenly to be coated it on kraft paper substrate with line rod spreader, and its coating thickness is 200 μ m.
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| CN102191003A (en) * | 2011-07-20 | 2011-09-21 | 常州合润新材料科技有限公司 | Silver-plated carbon nanotube heat-conducting adhesive and preparation method thereof |
| CN102634777B (en) * | 2012-02-23 | 2013-09-18 | 北京航空航天大学 | Electromagnetic shielding material for electroless cobalt plating of modified carbon nanotubes and preparation method of electromagnetic shielding material |
| CN108384177B (en) * | 2018-03-21 | 2020-06-23 | 成都工业学院 | Four-phase double-percolation electromagnetic shielding material and preparation method thereof |
| CN111312430A (en) * | 2020-02-25 | 2020-06-19 | 深圳市三顺纳米新材料股份有限公司 | Carbon nanotube conductive agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006114877A (en) * | 2004-09-15 | 2006-04-27 | Suzuki Sogyo Co Ltd | Electromagnetic wave absorption sheet, lamination thereof, and electromagnetic wave absorptivity housing using these |
| CN101285180A (en) * | 2008-01-11 | 2008-10-15 | 西北工业大学 | Process for preparing micro-coiled carbon fiber/Ni composite material by chemical nickel plating |
| CN101661858A (en) * | 2009-08-31 | 2010-03-03 | 福州大学 | Surface chemical metal plating carbon nanotube field-emission cathode preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006114877A (en) * | 2004-09-15 | 2006-04-27 | Suzuki Sogyo Co Ltd | Electromagnetic wave absorption sheet, lamination thereof, and electromagnetic wave absorptivity housing using these |
| CN101285180A (en) * | 2008-01-11 | 2008-10-15 | 西北工业大学 | Process for preparing micro-coiled carbon fiber/Ni composite material by chemical nickel plating |
| CN101661858A (en) * | 2009-08-31 | 2010-03-03 | 福州大学 | Surface chemical metal plating carbon nanotube field-emission cathode preparation method |
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