CN104124022A - Carbon-nanometer-tube-based magnetic nanometer composite material and manufacturing method thereof - Google Patents
Carbon-nanometer-tube-based magnetic nanometer composite material and manufacturing method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nanometer materials, in particular to a carbon-nanometer-tube-based magnetic nanometer composite material and a manufacturing method thereof. In the method, a nitrogen-doped carbon nanometer tube is manufactured by the adoption of a chemical vapor deposition method, then, ferromagnetic metal nanometer particles are loaded on the nitrogen-doped carbon nanometer tube through a solvothermal method, and therefore the carbon-nanometer-tube-based magnetic nanometer composite material is obtained. The carbon-nanometer-tube-based magnetic nanometer composite material and the manufacturing method have the advantages that raw materials needed in the manufacturing method are low in cost, the manufacturing technology is simple, and carbon-nanometer-tube-based magnetic nanometer composite materials can be manufactured on a large scale and are suitable for large-scale production and application. The obtained composite material is good in dispersity, and the magnetic metal nanometer particles are evenly distributed on the surface of the nitrogen-doped carbon nanometer tube (CNx) in a granular mode and are uniform in size.
Description
Technical field
The present invention relates to nano material synthesis technical field, more particularly, relate to a kind of carbon nanotube-based magnetic nanometer composite material and preparation method thereof.
Background technology
From 1991, Japanese S. Iijima found carbon nano-tube (Carbon nanotubes, CNTs) since, carbon nano-tube, with conductivity, thermal conductivity and unique magnetic performance of its unique one-dimensional nano structure, high draw ratio, the hardness that can match in excellence or beauty with diamond, high tenacity, excellence, is widely used in a plurality of fields such as Field Electron Emission, high-frequency wideband electro-magnetic wave absorption and heat conduction, Chu Qing and catalysis.
But carbon nano-tube exist easily assemble bunchy or winding, in most solvents the shortcoming of indissoluble, compare with other nano particles simultaneously, it is that every layer of nanotube is to pass through SP by a carbon atom by the curling seamless tubular shaped structure forming of single or multiple lift graphite
2the face of cylinder that hydridization and the hexagon plane that around three complete bondings of carbon atom form form, the integrated structure of its almost Perfect, hindered the intervention of foreign body and defect, make it have superpower mechanical property and very high chemical stability, therefore its chemism is even also low than graphite, shows relatively high chemical 'inertia'.These shortcomings have greatly restricted its extensive use above.
Therefore, the modifying surface of carbon nano-tube has been become one of the study hotspot of carbon nanotube-based material.For eliminating these restrictions, conventionally adopt the oxidants such as strong acid to carry out carbon nano-tube, make the oxygen-containing functional groups such as the Surface Creation hydroxyl of carbon pipe or carboxyl.Yet carbon pipe is carried out to oxidation processes meeting " is cut off " or " cutting off " carbon pipe, thereby change its original structure, affect its original performance.On the other hand, strong acid treatment mode has also produced negative effect to environment.Although and other method of modifying also can improve dispersiveness, hydrophily and the chemism of carbon nano-tube to a certain extent, also can weaken to a certain extent its other correlated performance.In recent years, by carbon nano-tube is carried out to ion doping, to improve the application performance of carbon nano-tube, become carbon nano-tube and synthesize one of study hotspot with application.Carbon nano-tube is adulterated and not only can be improved its dispersiveness, solve carbon nano-tube difficult shortcoming of disperseing in actual applications, and foreign atom can change carbon nano-tube partial charge density, the electronics transitivity of raising carbon nano-tube, reduction resistance coefficient.
CN
xbe the special material with carbon element that a class has tubular structure, it has the absorption property similar to common carbon pipe, mechanics, Thermodynamically stable performance.Meanwhile, with respect to carbon atom, nitrogen is than the many electronics of carbon, and these extra electronics can serve as charge carrier, thereby CN
xshow the semi-conductive general characteristic of n-type.In addition, owing to becoming extra electronics on single duplet and nitrogen-atoms, CN on N atom
xcan show the conjugation of enhancing and unique electricity and chemical property.On the one hand, pi-electron cloud, in the introducing of carbon nano tube surface, makes nitrogen doped carbon nanotube superficial layer present certain electronegativity, can be widely used in catalysis, inhale and involve the fields such as electronic device.On the other hand, CN
xn atom on framework can be used as chemism site, and then can in without surface-treated situation, realize metal, oxide and other semi-conducting materials etc. in the load of its carbon nano tube surface.Recently, thus the coated and load on nitrogen-doped carbon nanometer pipe surface such as metal, oxide forms the research of composite material has become an extremely important field.Ferromagnetic metal is the important soft magnetic material of a class, is mainly the Ferrious material in 3d magnesium-yttrium-transition metal, i.e. Fe, and Co, Ni and alloy thereof, it is widely used in electronic device, information storage, catalysis, the field such as stealthy.
Because the ferromagnetism of ferromagnetic metal derives from the 3d electronics that it is cruised; its saturation magnetic moment is determined by band structure; when the particle diameter of magnetic-particle is reduced to nanoscale; the reduction of its surface coordination number causes the variation of band structure, and the atomic magnetic moment of nano particle can change with the variation of particle size conventionally.In addition, the shape of magnetic-particle and structure also have material impact to its magnetic property, for example, by the control to magnetic-particle shape, can improve corresponding magnetic recording density, improve the DYNAMIC MAGNETIC of material.Therefore, ferromagnetic metal and nitrogen-doped carbon nanometer pipe are carried out compound, obtain the special novel micro nanometer rice magnetic composite of pattern and structure and its performance studied to the focus that becomes current research.Due to carbon nano-tube and the effect of ferromagnetic metal particle cooperative, at these composite materials, can demonstrate excellent enhancing effect.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of carbon nanotube-based magnetic nanometer composite material and preparation method thereof, its preparation technology is simple, with low cost.The carbon nanotube-based magnetic nanometer composite material obtaining has excellent properties.
In the present invention, adopt chemical vapour deposition technique to prepare nitrogen-doped carbon nanometer pipe, then use solvent-thermal method load iron magnetic metal nano particle on nitrogen doped carbon nanotube, thereby obtain carbon nanotube-based magnetic nanometer composite material.Concrete technical scheme is as follows.
The preparation method who the invention provides a kind of carbon nanotube-based magnetic nanometer composite material, concrete steps are as follows:
(1) preparation of nitrogen-doped carbon nanometer pipe CNx
The molecular sieve of processing is flooded in soluble iron salting liquid, and dry, roasting afterwards, obtains the carbon nano-tube catalyst for preparing of iron content; Under above-mentioned catalyst action, take organic amine as Carbon and nitrogen sources again, by chemical vapour deposition technique, prepare nitrogen-doped carbon nanometer pipe CNx;
(2) preparation of carbon nanotube-based magnetic nanometer composite material
1. nitrogen-doped carbon nanometer pipe CN step (1) being prepared
xwith NaOH or HF, process, remove wherein residual molecular sieve;
2. by the nitrogen-doped carbon nanometer pipe CN after above-mentioned processing
xjoin in solvent, sonic oscillation, fully disperses it, obtains suspension;
3. to the salt and the reducing agent that add solubility ferrous iron magnetic metal M in above-mentioned suspension, in closed container, carry out solvent heat treatment; Wherein: described M is selected from respectively one or more in Fe, Co or Ni; Described reducing agent is hydrazine hydrate; The reaction temperature of described solvent heat treatment is 200 ~ 220 ℃, and the reaction time is 2 ~ 4 hours;
Described nitrogen-doped carbon nanometer pipe material CN
xbe salt 0.0067 ~ 0.134mol/l of 0.02 ~ 0.2g, solubility ferrous iron magnetic metal M, volume 1 ~ 10 ml of hydrazine hydrate.
4. after reaction finishes, filter, washing, dryly obtain carbon nanotube-based magnetic nanometer composite material.
In above-mentioned steps (1), described soluble ferric iron salt is selected from, FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3, FeCl
2, FeSO
4or (NH
4)
2fe (SO
4)
2in one or more.
In above-mentioned steps (1), described organic amine is selected from ethylenediamine, diethylamine, methylamine, one or more in dimethylamine or pyridine.
In above-mentioned steps (1), described dry temperature is 100 ~ 150 ℃; The dry time is 8 ~ 20 hours; The temperature of described roasting is 500 ~ 850 ℃, and roasting time is 2 ~ 8 hours.
In above-mentioned steps (2), described solvent is selected from deionized water, ethylene glycol, isopropyl alcohol, one or more in glycerol or dimethyl formamide.
In above-mentioned steps (2), in the salt of described solubility ferrous iron ferromagnetic metal M, the divalent salts that contains Fe is selected from FeCl
2, FeSO
4or (NH
4)
2fe (SO
4)
2in any one or several; Divalent salts containing Co is selected from Co (NO
3)
2, CoCl
2, CoSO
4or Co (CH
3cOO)
2in any one or several, containing the divalent salts of Ni, be selected from Ni (NO
3)
2, NiCl
2, NiSO
4, Ni (CH
3cOO)
2and composition thereof; The concentration of the salt of solubility ferrous iron ferromagnetic metal M is 0.0067 ~ 0.134mol/L.
The present invention also provides a kind of carbon nanotube-based magnetic nanometer composite material obtaining according to above-mentioned preparation method.
Compared with prior art, beneficial effect of the present invention is:
1, in the present invention carbon nano-tube without functionalization in advance;
2, the required cost of raw material of preparation method provided by the invention is cheap;
3, preparation method provided by the invention does not need special consersion unit, does not need catalyst during heat treatment;
4, whole preparation process provided by the invention is removed outside carbon nano-tube preparation process, all under air conditions, carries out, without nitrogen protection;
5, the carbon nanotube-based magnetic nanometer composite material good dispersion for preparing of the present invention, ferromagnetic metal nano particle is evenly distributed in carbon nano tube surface, structured size.
Accompanying drawing explanation
Fig. 1 is ESEM (SEM) photo of the Ni/CNx nano composite material that makes of embodiment 1.
Fig. 2 is the Ni/CNx nano composite material M-H figure that embodiment 2 makes.
Embodiment
Below by specific embodiment, further illustrate the present invention.
embodiment 1the preparation of Ni/CNx nano composite material
(1), nitrogen-doped carbon nanometer pipe material (CN
x) preparation:
By 10 g soluble ferric iron salt FeCl
3be dissolved in deionized water; Then dropwise join in the NaY molecular sieve that 10 g processed and flood, after, at 100 ~ 150 ℃ of temperature dry 8 hours, then 850 ℃ of roasting temperatures 2 hours, obtain the carbon nano-tube catalyst for preparing of iron content; Take ethylenediamine as Carbon and nitrogen sources again, under the catalyst action making, with the flow velocity of 20mL/min, 650 ~ 1000 ℃ of process chemical vapor deposition (CVD) design temperatures, constant temperature 0.5 ~ 5 hour, obtains nitrogen-doped carbon nanometer pipe material (CN
x);
(2), the preparation of Ni/CNx nano composite material
1. nitrogen-doped carbon nanometer pipe CN step (1) being prepared
xin HF solution, stir 30min,, remove wherein residual molecular sieve;
2. by the nitrogen-doped carbon nanometer pipe CN after above-mentioned processing
xjoin in ethylene glycol, sonic oscillation, fully disperses it, and the concentration that obtains 40 mL is the suspension of 0.5 g/L;
3. in above-mentioned suspension, add 0.3 mmol Ni (NO
3)
2with 2 ml hydrazine hydrates, in closed container, carry out solvent heat treatment, its reaction temperature is 200 ℃, the reaction time is 4 hours;
4. after reaction finishes, filter, with deionized water, ethanol washing, then vacuumize obtains Ni/CNx nano composite material; Scanning electron (SEM) photo of Ni/CNx nano composite material prepared by the present embodiment as shown in Figure 1.The carbon nano tube surface of the sample overwhelming majority making is as can be seen from Figure 1 coated by metal Ni completely, only have only a few carbon nano-tube by Ni, not to be coated, the coated carbon nano-tube of Ni presents exclusive cable shape structure, with respect to not coated carbon nano-tube, Ni/CN
xthe diameter of nano composite material obviously increases thick, and surface does not have coated carbon nano-tube coarse yet.These Ni nano-particles size distribute comparatively even, and particle diameter is between tens nanometers.
embodiment 2
By the soluble ferric iron salt FeCl in the step of embodiment 1 (1)
3with Fe (NO
3)
3, replacing, other steps and condition are all identical with embodiment 1, can obtain Ni/CNx nano composite material equally.Its Ni/CNx nano composite material M-H figure as shown in Figure 2.Therefrom can find out at applying a magnetic field to be that 8000 Oe left and right have reached saturated substantially, and saturation magnetization (
m s) higher, surpass 50 emu/g a little less than the metal Ni block structure of pure phase.。
embodiment 3
Ethylenediamine in the step of embodiment 1 (1) is replaced with dimethylamine, and other steps and condition are all identical with embodiment 1, can obtain Ni/CNx nano composite material equally.
embodiment 4
Ni (NO in the step of embodiment 1 (2)
3)
2with other Ni salt, Fe salt and Co salt, replace, other Ni salt comprise NiCl
2, NiSO
4, Ni (CH
3cOO)
2and composition thereof; Fe salt, comprises FeCl
2, FeSO
4, (NH
4)
2fe (SO
4)
2and composition thereof; Co salt, comprises Co (NO
3)
2, CoCl
2, CoSO
4, Co (CH
3cOO)
2and composition thereof replace Ni (NO
3)
2, other steps are all similar to embodiment 1 with condition, do corresponding change and adjust in the scope that actual conditions limits at summary of the invention, can obtain equally Ni/CNx nano composite material, Fe/CNx nano composite material, Co/CNx nano composite material.
embodiment 5
Except the divalent salts of the use in step (2) containing Ni, comprise NiCl
2, NiSO
4, Ni (CH
3cOO)
2and composition thereof; Divalent salts containing Fe, comprises FeCl
2, FeSO
4, (NH
4)
2fe (SO
4)
2and composition thereof; Divalent salts containing Co, comprises Co (NO
3)
2, CoCl
2, CoSO
4, Co (CH
3cOO)
2and composition thereof, therefrom any two kinds replace Ni (NO
3)
2, other steps are all similar to embodiment 2 with condition, do corresponding change and adjust in the scope that actual conditions limits at summary of the invention, obtain equally NiCo/CNx nano composite material, FeCo/CNx nano composite material, FeNi/CNx nano composite material.
embodiment 6
In embodiment 6, except the divalent salts containing Ni for step (2), comprise NiCl
2, NiSO
4, Ni (CH
3cOO)
2and composition thereof; Divalent salts containing Fe, comprises FeCl
2, FeSO
4, (NH
4)
2fe (SO
4)
2and composition thereof; Divalent salts containing Co, comprises Co (NO
3)
2, CoCl
2, CoSO
4, Co (CH
3cOO)
2and composition thereof, therefrom choose arbitrarily divalent salts containing Ni, containing the divalent salts of Fe and containing the divalent salts of Co totally three kinds replace Ni (NO
3)
2, other steps are all similar to embodiment 3 with condition, do corresponding change and adjust in the scope that actual conditions limits at summary of the invention, obtain equally FeCoNi/CNx nano composite material.
Claims (7)
1. a preparation method for carbon nanotube-based magnetic nanometer composite material, is characterized in that, comprises the following steps:
(1) preparation of nitrogen-doped carbon nanometer pipe CNx
NaY molecular sieve after calcining is placed in to soluble iron salting liquid and floods, dry, roasting afterwards, obtains the carbon nano-tube catalyst for preparing of iron content; Under above-mentioned catalyst action, take organic amine as Carbon and nitrogen sources again, by chemical vapour deposition technique, prepare nitrogen-doped carbon nanometer pipe CNx;
(2) preparation of carbon nanotube-based magnetic nanometer composite material
1. nitrogen-doped carbon nanometer pipe CN step (1) being prepared
xwith NaOH or HF, process, remove wherein residual molecular sieve;
2. by the nitrogen-doped carbon nanometer pipe CN after above-mentioned processing
xjoin in solvent, sonic oscillation, fully disperses it, obtains suspension;
3. to the salt and the hydrazine hydrate that add solubility ferrous iron magnetic metal M in above-mentioned suspension, in closed container, carry out solvent heat treatment; Wherein: described M is selected from respectively one or more in Fe, Co or Ni; The reaction temperature of described solvent heat treatment is 200 ~ 220 ℃, and the reaction time is 2 ~ 4 hours; Described nitrogen-doped carbon nanometer pipe material CN
xbe salt 0.0067 ~ 0.134mol/l of 0.02 ~ 0.2g, solubility ferrous iron magnetic metal M, volume 1 ~ 10 ml of hydrazine hydrate;
4. after reaction finishes, filter, washing, dryly obtain carbon nanotube-based magnetic nanometer composite material.
2. preparation method according to claim 1, is characterized in that: in step (1), described soluble ferric iron salt is selected from, FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3, FeCl
2, FeSO
4or (NH
4)
2fe (SO
4)
2in one or more.
3. preparation method according to claim 1, is characterized in that: in step (1), described organic amine is selected from ethylenediamine, diethylamine, methylamine, one or more in dimethylamine or pyridine.
4. preparation method according to claim 1, is characterized in that: in step (1), described dry temperature is 100 ~ 150 ℃; The dry time is 8 ~ 20 hours; The temperature of described roasting is 500 ~ 850 ℃, and roasting time is 2 ~ 8 hours.
5. preparation method according to claim 1, is characterized in that: in step (2), described solvent is selected from deionized water, ethylene glycol, isopropyl alcohol, one or more in glycerol or dimethyl formamide.
6. preparation method according to claim 1, is characterized in that: in step (2), in the salt of described solubility ferrous iron ferromagnetic metal M, the divalent salts that contains Fe is selected from FeCl
2, FeSO
4or (NH
4)
2fe (SO
4)
2in any one or several; Divalent salts containing Co is selected from Co (NO
3)
2, CoCl
2, CoSO
4or Co (CH
3cOO)
2in any one or several, containing the divalent salts of Ni, be selected from Ni (NO
3)
2, NiCl
2, NiSO
4, Ni (CH
3cOO)
2and composition thereof; The concentration of the salt of solubility ferrous iron ferromagnetic metal M is 0.0067 ~ 0.134mol/L.
7. the carbon nanotube-based magnetic nanometer composite material that preparation method according to claim 1 obtains.
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| CN112087939A (en) * | 2020-09-10 | 2020-12-15 | 中山大学 | FeCoNi @ C/carbon nanotube magnetic composite wave-absorbing material and preparation method and application thereof |
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| CN114538433A (en) * | 2022-02-25 | 2022-05-27 | 中南大学 | Method for preparing quick-charging graphite with single-metal-doped defects |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109448947A (en) * | 2018-10-26 | 2019-03-08 | 同济大学 | A kind of carbon nano tube-doped iron-based soft magnetic composite powder and preparation method thereof |
| CN111135788A (en) * | 2019-09-18 | 2020-05-12 | 青岛农业大学 | Magnetic nitrogen-doped carbon nanotube water treatment adsorbent and preparation method thereof |
| CN112087939A (en) * | 2020-09-10 | 2020-12-15 | 中山大学 | FeCoNi @ C/carbon nanotube magnetic composite wave-absorbing material and preparation method and application thereof |
| CN113265223A (en) * | 2021-05-24 | 2021-08-17 | 西北工业大学 | Nitrogen-doped iron-carbon composite wave-absorbing material and preparation method and application thereof |
| CN114225952A (en) * | 2021-11-09 | 2022-03-25 | 华南理工大学 | Magnetic nitrogen-doped carbon nanotube and preparation method and application thereof |
| CN114538433A (en) * | 2022-02-25 | 2022-05-27 | 中南大学 | Method for preparing quick-charging graphite with single-metal-doped defects |
| CN114538433B (en) * | 2022-02-25 | 2023-11-10 | 中南大学 | Method for preparing quick graphite filling with single metal doping defect |
| CN115124478A (en) * | 2022-06-27 | 2022-09-30 | 海南华瑞医药有限公司 | Iron-nitrogen co-doped carbon material catalyst and application thereof in synthesis of quinazoline and derivatives thereof |
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Effective date of registration: 20210203 Address after: Room 208, building 6, 199 Tongji Branch Road, Baoshan District, Shanghai, 200940 Patentee after: SHANGHAI JIANLING ENERGY SAVING AND ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Address before: 202161 no.4925 Chenzhao Road, Xianghua Town, Chongming District, Shanghai (Shanghai Yongguan Economic Development Zone) Patentee before: Shanghai Iguazu Environmental Protection Technology Service Center |
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Effective date of registration: 20211206 Address after: 201900 Building 1, No. 2, Tongji Road, Baoshan District, Shanghai Patentee after: Jianling environmental protection technology (Shanghai) Co.,Ltd. Address before: Room 208, building 6, 199 Tongji Branch Road, Baoshan District, Shanghai, 200940 Patentee before: SHANGHAI JIANLING ENERGY SAVING AND ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. |
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