CN101118796A - One-dimensional nano magnetic materials manufacturing method based on nano carbon tube - Google Patents
One-dimensional nano magnetic materials manufacturing method based on nano carbon tube Download PDFInfo
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- CN101118796A CN101118796A CNA2007100522285A CN200710052228A CN101118796A CN 101118796 A CN101118796 A CN 101118796A CN A2007100522285 A CNA2007100522285 A CN A2007100522285A CN 200710052228 A CN200710052228 A CN 200710052228A CN 101118796 A CN101118796 A CN 101118796A
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Abstract
The present invention relates to a one-dimensional nanometer-sized magnetic material production method which is based on carbon nanotubes, and is characterized in that firstly, pretreatment of carbon nanotubes is carried before nickel-cobalt plating, and relatively pure carbon tubes are obtained through purification and oxidation, and then catalytic metal cores are formed on the surface of carbon nanotubes by dint of activation and sensitization; secondly, the pretreated carbon nanotubes are added to Co-P, Co-Ni-P, Co-Fe-P Cobalt-based alloy plating solution and the reaction process gets decentralized by ultrasonic oscillations. The method has the advantages of little damage to carbon nanotube, easy operation, simple production technique, low cost, and easy preparation; and also has the capability of excellent uniform plating and deep plating; thus being suitable for the surface plated treatment of carbon nanotube. After the treatments, the coercive force and the saturation magnetic density of carbon nanotube are improved a lot. Compared with thin-film plating, coarse power and large alloy blocks, the coercive force of carbon nanotube being plated with Co-P and Co-Ni-P is improved significantly.
Description
Technical field
The present invention relates to a kind of manufacture method of the 1-dimention nano magnetic material based on CNT (carbon nano-tube).
Background technology
The CNT (carbon nano-tube) functional material of processability excellence is the focus and emphasis of material area research, and it is very important to set up reliable synthetic method.Major opportunity and challenge that the development of the nanosecond science and technology of nearly decades has brought great-leap-forward development for traditional magnetic material industry make this field become one of at present noticeable and the most most active in the world research field.
The electroless cobalt plating layer of elements such as phosphorous, boron has good magnetic memory function, rectifys stupid coefficient height, has wide practical use in fields such as the magnetic holder of computer and electronic instrumentss.Because the needs of electronics industry development are a lot of to the research of chemical plating magnetic film technology both at home and abroad, but less in the relevant report of CNT (carbon nano-tube) surface cobalt plating at present.Electroless deposited co-ni has had the advantage of chemical plating Co-P and chemical Ni-P plating concurrently.Has good resistance to wear, corrosion resistance and soft or hard magnetic.The Co-Ni-P alloy firm has higher coercive force, and less remanent magnetism and good electromagnetic conversion characteristics can be used as compact disk and magnetic sound recording system.Abroad be widely used on the speed-sensitive switch element of highdensity memory cell of high-quality and electronic computer storage device at present.Electroless cobalt plating---phosphorus based multicomponent alloy coating generally all has good electromagnetic performance, and what have also has an electric catalyticing characteristic, thereby is subject to people's attention.Add a certain amount of molysite and complexing agent in cobalt-phosphorus alloy plating liquid, under suitable condition, just can deposit the Co-Fe-P alloy layer.This alloy layer also has electromagnetic performance preferably.At present, yet there are no the relevant report of CNT (carbon nano-tube) coating surface ferro-cobalt.
Can on light carrier, coat the lightweight magnetic material that the last layer magnetisable material makes a kind of novelty with methods such as chemical plating, vapour deposition, sol-gel techniques.This method gives material new characteristic, has widened the kind and the application of magnetic material.Chemical nickel plating on powdered graphite can be used as electric conducting material and microwave absorbing material; Chemical nickel plating or nickel-cobalt alloy on the CNT (carbon nano-tube) can be used as microwave absorbing material and recording materials; At carbon fiber surface coating BaFe
12O
10Type ferrite can be used on the microwave absorbing coating; At metal such as hollow glass micro-ball surface vapour deposition Fe, Ti or Electroless Plating Ni, metals such as Co, Ni-Fe, can be used on microwave absorbing material and the medical immunology detection technique.
The research of lightweight magnetic material be of magnetic material research the preparation method is more than frontier, but many technology are still waiting to improve.Wherein, the method that light carrier is coated just can obtain even, scattered lightweight magnetic material as long as carrier is selected proper and method for coating is suitable.Vapour deposition and sol-gel technique need expensive equipment or complicated technology in the method that coats, and the electroless plating technology process equipment is simple, and be easy to operate, can be fit to complex-shaped object.At present, the research of adopting electroless plating technology to prepare the lightweight magnetic material has caused scholars' extensive concern.
The present invention adopts a kind of simple method to modify CNT (carbon nano-tube) first, produces more desirable magnetic property when making CNT (carbon nano-tube) keep its original character again.
Summary of the invention
The technical problem to be solved in the present invention is, original CNT (carbon nano-tube) surface is with carbon polyhedral nano particles, carbon onion, and impurity such as amorphous carbon, makes it uneven.Because the CNT (carbon nano-tube) surface curvature is big, be difficult for plating again, uneven coating is even, and tack is poor; And the CNT (carbon nano-tube) diameter is thinner, difficulties in dispersion, and its carbonization structure also makes its reactivity extremely low, is difficult to obtain the good coating of continuity compactness.
The objective of the invention is: the manufacture method that a kind of 1-dimention nano magnetic material based on CNT (carbon nano-tube) is provided, destruction to CNT (carbon nano-tube) is very little, easy to operate, technology is simple, with low cost, easily preparation, and this method operation also has good all platings and covering power, and the coating surface that therefore is well suited for CNT (carbon nano-tube) is handled.
The technical solution adopted in the present invention is: a kind of manufacture method of the 1-dimention nano magnetic material based on CNT (carbon nano-tube), it is characterized in that: a. at first carried out preliminary treatment to CNT (carbon nano-tube) before the nickel plating cobalt, obtain purer CNT (carbon nano-tube) by purifying, oxidation processes, handle on the CNT (carbon nano-tube) surface forming catalytic metal nuclear again by activation, sensitization; B. pretreated CNT (carbon nano-tube) is added in Co-P, Co-Ni-P, the Co-Fe-P cobalt-base alloys plating bath, course of reaction is disperseed with supersonic oscillations;
Concrete steps are as follows:
At first CNT (carbon nano-tube) is carried out purification process, CNT (carbon nano-tube) is dropped into the NaOH aqueous solution that concentration is 1-3mol/L, vibration fully disperses in ultrasonic oscillator, and ultrasonic power is every ultrasonic 30 seconds, stops 30 seconds; Heated 0.2-2 hour, and be cooled to room temperature; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
The 5-15 of purified processing gram CNT (carbon nano-tube) added in the 250mL red fuming nitric acid (RFNA) carry out oxidation processes, be heated to more than 60 ℃ 5-0 minute; Vibration fully disperses in ultrasonic oscillator, leaves standstill 20-30 hour; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
CNT (carbon nano-tube) through oxidation processes is carried out the sensitization activation processing: at room temperature, the CNT (carbon nano-tube) of 0.2-2 gram after oxidation added the 400ml sensitizing solution, and (2-8 restrains SnCl
22H
20+37.66mlHCl) in, utilize ultrasonic oscillator fully to disperse; After the filtration, it is added the 400ml activating solution, and (0.05-0.5 restrains PdCl
2+ 17.2mlHCl) in, utilize ultrasonic oscillator fully to disperse, reaction finish the back with washed with de-ionized water to neutral.
Based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that as mentioned above: add 0.005-0.05 gram CNT (carbon nano-tube) in every 100mL plating bath, course of reaction is fully disperseed with ultrasonic oscillator.
Based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that as mentioned above: best useful load is to add 0.01-0.03 gram CNT (carbon nano-tube) in 100 milliliters of plating baths during plating.This moment, plating bath disperseed better, and the thickness phenomenon does not appear in plating bath in the plating process.
Based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that: described cobalt-base alloys plating bath is as mentioned above:
Table 1 cobalt plating phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 15-25 |
| NaH 2PO 2·H 2O | 20-30 |
| KNaC 4H 4O 4·4H 2O | 130-140 |
| (NH4) 2SO 4 | 60-65 |
| PH value | 8.8～9.0 |
| Temperature (℃) | 65-70 |
Table 2 cobalt plating nickel phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 20-25 |
| NiSO 4·7H 2O | 4.5-5.0 |
| NaH 2PO 2·H 2O | 25.4-26.0 |
| KNaC 4H 4O 4·4H 2O | 43-45 |
| (NH4) 2SO 4 | 23-25 |
| PH value | 9.0～9.5 |
| Temperature (℃) | 50-55 |
Table 3 cobalt plating iron phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 24-26 |
| (FeSO 4) 2·7H 2O | 1.2-2.0 |
| NaH 2PO 2·H 2O | 35-45 |
| KNaC 4H 4O 4·4H 2O | 28-32 |
| (NH4) 2SO 4 | 38-42 |
| PH value | 8.2-8.9 |
| Temperature (℃) | 65-70 |
Adopt this method very little to the destruction of CNT (carbon nano-tube), easy to operate, technology is simple, and is with low cost, easily preparation, and this method operation also has good all platings and covering power.Therefore the coating surface that is well suited for CNT (carbon nano-tube) is handled.The deposition velocity of parent metal can obtain low-phosphorous magnetic composite deposite in the control plating process.
Embodiment
The processing step of multiple-wall carbon nanotube chemical nickel plating on surface cobalt is as follows:
1. purification process: adopt alkali lye to remove CNT (carbon nano-tube) surface fat metallic substance.CNT (carbon nano-tube) is dropped into the NaOH aqueous solution that concentration is 1-3mol/L, and vibration fully disperses in ultrasonic oscillator, and ultrasonic power is every ultrasonic 30 seconds, stops 30 seconds; Heated 0.2-2 hour, and be cooled to room temperature; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
Value is preferably: CNT (carbon nano-tube) is dropped into the NaOH aqueous solution that concentration is 2mol/L, and vibration fully disperses in ultrasonic oscillator, and ultrasonic power is every ultrasonic 30 seconds, stops 30 seconds; Heated 1 hour, and be cooled to room temperature.
2. the 5-15 of purified processing gram CNT (carbon nano-tube) is added in the 250mL red fuming nitric acid (RFNA) and carry out oxidation processes, be heated to more than 60 ℃ 5-60 minute; Vibration fully disperses in ultrasonic oscillator, leaves standstill 20-30 hour; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
Value is preferably: 10 gram CNT (carbon nano-tube) are gone into to carry out oxidation processes in the 250mL red fuming nitric acid (RFNA), be heated to more than 60 ℃ 15 minutes; Vibration fully disperses in ultrasonic oscillator, leaves standstill 24 hours.
3. sensitization activation processing: the CNT (carbon nano-tube) through oxidation processes is carried out the sensitization activation processing: at room temperature, the CNT (carbon nano-tube) of 0.2-2 gram after oxidation added the 400ml sensitizing solution, and (2-8 restrains SnCl
22H
2O+37.66mlHCl) in, utilize ultrasonic oscillator fully to disperse; After the filtration, it is added the 400ml activating solution, and (0.05-0.5 restrains PdCl
2+ 17.2mlHCl) in, utilize ultrasonic oscillator fully to disperse, reaction finish the back with washed with de-ionized water to neutral.
Value is preferably: 1 gram is added 400ml sensitizing solution (4 gram SnCl through the CNT (carbon nano-tube) of oxidation
22H
2O+37.66mlHCl) in, utilize ultrasonic oscillator fully to disperse; After the filtration, it is added 400ml activating solution (0.19 gram PdCl
2+ 17.2ml HCl) in.
4. pretreated CNT (carbon nano-tube) is added respectively in Co-P, Co-Ni-P, the Co-Fe-P cobalt-base alloys plating bath of following table prescription, useful load is to add 0.005-0.05 gram CNT (carbon nano-tube) in every 100mL plating bath, and course of reaction is fully disperseed with ultrasonic oscillator.
Best useful load is to add 0.01-0.03 gram CNT (carbon nano-tube) in 100 milliliters of plating baths during plating.This moment, plating bath disperseed better, and the thickness phenomenon does not appear in plating bath in the plating process.
Table 1 cobalt plating phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 15-25 |
| NaH 2PO 2·H 2O | 20-30 |
| KNaC 4H 4O 4·4H 2O | 130-140 |
| (NH4) 2SO 4 | 60-65 |
| PH value | 8.8～9.0 |
| Temperature (℃) | 65-70 |
Table 2 cobalt plating nickel phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 20-25 |
| NiSO 4·7H 2O | 4.5-5.0 |
| NaH 2PO 2·H 2O | 25.4-26.0 |
| KNaC 4H 4O 4·4H 2O | 43-45 |
| (NH4) 2SO 4 | 23-25 |
| PH value | 9.0～9.5 |
| Temperature (℃) | 50-55 |
Table 3 cobalt plating iron phosphorus component and condition
| Prescription | Component content (g/L) |
| CoSO 4·7H 2O | 24-26 |
| (FeSO 4) 2·7H 2O | 1.2-2.0 |
| NaH 2PO 2·H 2O | 35-45 |
| KNaC 4H 4O 4·4H 2O | 28-32 |
| (NH4) 2SO 4 | 38-42 |
| PH value | 8.2-8.9 |
| Temperature (℃) | 65-70 |
Utilize the transmission electron microscope observing contrast to plate front and back and heat treatment front and back coating morphology, can see continuous, the densification, smooth of plating back CNT (carbon nano-tube) outer surface composite deposite, the clad ratio height coats complete.Illustrate that this method cobalt plating base alloy has stronger covering power.Coating is continuous, fine and close, smooth after the heat treatment.With the composition of electron spectroscopy analysis test coating, coating surface has Co-P, Co-Ni-P, Co-Fe-P cobalt-base alloys element to exist respectively as can be known.At CNT (carbon nano-tube) coating surface longitudinal scanning, during scanning nano carbon tube-surface chemical plating Co-P, high-visible have the cobalt element energy level to jump obviously, and the cobalt distribution uniform by electron beam.Cobalt content is higher, accounts for 99.04%; And phosphorus only accounts for 0.96%; During scanning nano carbon tube-surface electroless deposited co-ni, cobalt element and nickel element energy level jump high-visible, and cobalt and nickel distribution uniform.Cobalt content is higher, accounts for 82.14%; Nickel takes second place, and accounts for 16.43%; And phosphorus only accounts for 1.43%; During scanning nano carbon tube-surface chemical plating Co-Fe-P, high-visible have the energy level of cobalt and ferro element to jump very obviously and distribution uniform.Cobalt content is higher, accounts for 95.08%; Iron content is lower, accounts for 4.4%; And phosphorus only accounts for 0.52%.Carbon nano-tube Ni-P coating, Co-P coating, Co-Ni-P coating, Co-Fe-P composite deposite before and after the heat treatment are carried out magnetic property research.Vibration magnetic strength detector test result shows: the pure nano-carbon tube coercive force is 146Oe, and specific saturation magnetization is 1.9393emu/g; The coercive force of CNT (carbon nano-tube) reaches 692.61Oe behind the cobalt plating phosphorus, and specific saturation magnetization is 132.9504emu/g; The coercive force of CNT (carbon nano-tube) reaches 166Oe behind the cobalt plating nickel phosphorus, and specific saturation magnetization is 89.1386emu/g; The coercive force of carbon nano-tube can reach 467.71Oe behind the cobalt plating iron phosphorus, and specific saturation magnetization can reach 114.9359emu/g.As seen plating back coercive force and specific saturation magnetization are more a lot of than having improved before plating.With thin film coating, meal and bulk alloy phase ratio, the coercive force of CNT (carbon nano-tube) has no small amplification behind cobalt plating phosphorus and the cobalt plating nickel phosphorus, and this is the new effect that nano-scale brings.
Claims (4)
1. manufacture method based on the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that: a. at first carried out preliminary treatment to CNT (carbon nano-tube) before the nickel plating cobalt, obtain purer CNT (carbon nano-tube) by purifying, oxidation processes, handle on the CNT (carbon nano-tube) surface forming catalytic metal nuclear again by activation, sensitization; B. pretreated CNT (carbon nano-tube) is added in Co-P, Co-Ni-P, the Co-Fe-P cobalt-base alloys plating bath, course of reaction is disperseed with supersonic oscillations;
Concrete steps are as follows:
At first CNT (carbon nano-tube) is carried out purification process, CNT (carbon nano-tube) is dropped into the NaOH aqueous solution that concentration is 1-3mol/L, vibration fully disperses in ultrasonic oscillator, and ultrasonic power is every ultrasonic 30 seconds, stops 30 seconds; Heated 0.2-2 hour, and be cooled to room temperature; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
The 5-15 of purified processing gram CNT (carbon nano-tube) added in the 250mL red fuming nitric acid (RFNA) carry out oxidation processes, be heated to more than 60 ℃ 5-60 minute; Vibration fully disperses in ultrasonic oscillator, leaves standstill 20-30 hour; Extremely neutral with deionized water wash; The powder of cleaning is placed the vacuum drying chamber drying;
CNT (carbon nano-tube) through oxidation processes is carried out the sensitization activation processing: at room temperature, the CNT (carbon nano-tube) of 0.2-2 gram after oxidation added in the 400ml sensitizing solution, the component of sensitizing solution: 2-8 restrains SnCl
22H
2O+37.66mlHCl utilizes ultrasonic oscillator fully to disperse; After the filtration, it is added in the 400ml activating solution component 0.05-0.5 of activating solution gram PdCl
2+ 17.2mlHCl utilizes ultrasonic oscillator fully to disperse, and it is extremely neutral with washed with de-ionized water that reaction finishes the back.
2. according to claim 1 based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that: add 0.005-0.05 gram CNT (carbon nano-tube) in every 100mL plating bath, course of reaction is fully disperseed with ultrasonic oscillator.
As described in the claim 2 based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that: best useful load is to add 0.01-0.03 gram CNT (carbon nano-tube) in 100 milliliters of plating baths during plating.
As described in claim 1 or 2 or 3 based on the manufacture method of the 1-dimention nano magnetic material of CNT (carbon nano-tube), it is characterized in that: described cobalt-base alloys plating bath is:
1. cobalt plating phosphorus Co-P component and condition
Formula components content g/L
CoSO
4·7H
2O 15-25
NaH
2PO
2·H
2O 20-30
KNaC
4H
4O
4·4H
2O 130-140
(NH4)
2SO
4 60-65
PH value 8.8～9.0 temperature 65-70 ℃;
2. cobalt plating nickel phosphorus Co-Ni-P component and condition
Formula components content g/L
CoSO
4·7H
2O 20-25
NiH
2PO
2·H
2O 4.5-5.0
NaH
2PO
2·H
2O 25.4-26.0
KNaC
4H
4O
4·4H
2O 43-45
(NH4)
2SO
4 23-25
PH value 9.0～9.5, temperature 50-55 ℃;
3. cobalt plating iron phosphorus Co-Fe-P component and condition
Formula components content g/L
CoSO
4·7H
2O 24-26
(FeSO
4)
2·7H
2O 1.2-2.0
NaH
2PO
2·H
2O 35-45
KNaC
4H
4O
4·4H
2O 28-32
(NH4)
2SO
4 38-42
PH value 8.2～8.9, temperature 65-70 ℃.
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| CNA2007100522285A CN101118796A (en) | 2007-05-23 | 2007-05-23 | One-dimensional nano magnetic materials manufacturing method based on nano carbon tube |
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|---|---|---|---|
| CNA2007100522285A CN101118796A (en) | 2007-05-23 | 2007-05-23 | One-dimensional nano magnetic materials manufacturing method based on nano carbon tube |
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ID=39054855
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101976594A (en) * | 2010-08-31 | 2011-02-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Composite conductor application of carbon nano tube fiber and preparation method thereof |
| CN105458292A (en) * | 2015-12-10 | 2016-04-06 | 北京理工大学 | Preparation method of carbon nano tube/copper powder |
| CN106270500A (en) * | 2016-09-30 | 2017-01-04 | 昆明理工大学 | A kind of carbon nano tube surface is uniformly coated with the method and device of argent |
-
2007
- 2007-05-23 CN CNA2007100522285A patent/CN101118796A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101976594A (en) * | 2010-08-31 | 2011-02-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Composite conductor application of carbon nano tube fiber and preparation method thereof |
| CN105458292A (en) * | 2015-12-10 | 2016-04-06 | 北京理工大学 | Preparation method of carbon nano tube/copper powder |
| CN106270500A (en) * | 2016-09-30 | 2017-01-04 | 昆明理工大学 | A kind of carbon nano tube surface is uniformly coated with the method and device of argent |
| CN106270500B (en) * | 2016-09-30 | 2019-02-19 | 昆明理工大学 | A kind of carbon nano tube surface uniformly coats the method and device of metallic silver |
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