CN100368080C - Method for preparing carbon nanotubes and carbon onions by Ni/Al catalyst chemical vapor deposition - Google Patents
Method for preparing carbon nanotubes and carbon onions by Ni/Al catalyst chemical vapor deposition Download PDFInfo
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- CN100368080C CN100368080C CNB200510014889XA CN200510014889A CN100368080C CN 100368080 C CN100368080 C CN 100368080C CN B200510014889X A CNB200510014889X A CN B200510014889XA CN 200510014889 A CN200510014889 A CN 200510014889A CN 100368080 C CN100368080 C CN 100368080C
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 241000234282 Allium Species 0.000 title claims abstract description 34
- 235000002732 Allium cepa var. cepa Nutrition 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract 7
- 239000002041 carbon nanotube Substances 0.000 title claims abstract 7
- 239000011203 carbon fibre reinforced carbon Substances 0.000 title claims abstract 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000004523 catalytic cracking Methods 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims abstract 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims 2
- 229910018590 Ni(NO3)2-6H2O Inorganic materials 0.000 claims 1
- 229910018661 Ni(OH) Inorganic materials 0.000 claims 1
- 241001674048 Phthiraptera Species 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000004411 aluminium Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 5
- 239000003595 mist Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- -1 carbon ion Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The present invention discloses a method for preparing carbon nanotubes and carbon onions by the chemical vapor deposition of a Ni/Al catalyst. The prepared carbon nanotubes and the prepared carbon onions has the advantages of good quality, high purity and large yield. The present invention firstly uses nickel nitrate hexahydrate and aluminium powder with a certain weight ratio and uses sodium hydroxide or ammonia water as a precipitating agent to prepare Ni/Al catalyst precursor with a corresponding weight ratio; before catalytic cracking reaction is carried out, hydrogen gas is led in to reduce the catalyst precursor to the Ni/Al catalyst; then, methane or acetylene, etc. are led in as a carbon source to carry out the catalytic cracking reaction for 1 to 4 hours.
Description
Technical field
The present invention relates to the technology of preparing of a kind of CNT and carbon onion.
Background technology
CNT has been a kind of new function material and structural material of excellent performance by generally acknowledging in the world, can be used as high density hydrogen storage material, high strength composite, fine definition FPD, nanometer apparatus and electromagnet absorbing material etc.At present, the method for preparing CNT mainly contains three kinds of catalystic pyrolysis, arc process and laser evaporation methods.Prepare CNT with catalystic pyrolysis and need use transition metal (Fe, Co, Ni) or its compound as catalyst usually.Though with Ni/Al
2O
3It is comparatively ripe to do the development of Preparation of Catalyst CNT, its output height, and the purity height, but the carbon pipe that obtains is owing to must be not suitable for being applied to composite through complicated purification step.Be equipped with CNT and make catalyst CVD legal system, had not yet to see bibliographical information with Ni/Al.
The carbon onion is a kind of new function material and structural material of excellent performance, can be used as single-electron device, low temperature magnetic refrigerator, nanotube diode, nano-transistor, nano bearing and insulator lubricant etc.At present, the method for preparing the carbon onion heat treating process, the carbon ion that mainly contain arc process, high-energy irradiation method, material with carbon element injects the metal method and plasma strengthens catalystic pyrolysis etc.Said method is temperature required height in preparation carbon onion process, and energy is big.At present, prepare the carbon onion with the CVD method, bibliographical information just with Ni as catalyst, in the carbon products that in the end obtains, the carbon onion is few, therefore complicated separation and the purification step that is absolutely necessary.
Summary of the invention
The object of the present invention is to provide the method for a kind of efficient easy manufacture CNT and carbon onion.The complex catalyst precursor preparation process of this method is simple; The productive rate of CNT and carbon onion is big, purity is high; Gained carbon pipe caliber is less and even, and caliber is controlled; Gained carbon onion particle diameter is less and very even, the kernel cleaning.
The present invention is achieved through the following technical solutions, and step comprises:
1) preparation Ni/Al catalyst precursor:
With six water nickel nitrates and aluminium powder is Ni (NO by weight
3)
26H
2O: Al=0.127-193.1: 1 joins in the distilled water, the solution concentration that makes gained six water nickel nitrates is 0.1mol/L, make precipitating reagent with NaOH or ammoniacal liquor, drip precipitating reagent to solution under stirring and be neutral, obtaining nickel aluminium weight ratio is Ni/Al=0.025-39: 1 Ni (OH)
2/ Al binary colloidal; This binary colloidal is dewatered under 150 ℃-300 ℃, nitrogen atmosphere, and, obtain the Ni/Al catalyst precursor of corresponding weight score at 350 ℃ of-500 ℃ of temperature lower calcinations;
2) preparation CNT and carbon onion
Getting step 1) gained nickel aluminium weight ratio is Ni/Al=0.025-0.67: 1 and Ni/Al=1.5-39: the Ni/Al catalyst precursor of two kinds of weight scores of 1 is layered in the quartz boat; Quartz boat is placed flat-temperature zone, crystal reaction tube middle part; Feed the air in the nitrogen drain, be warming up to 500 ℃-650 ℃ then; Feed hydrogen, and keep hydrogen to pass through catalyst precursor 1.5-4 hour, stop hydrogen with the flow velocity of 25mL/min-250mL/min; Feed methane or acetylene reaction gas afterwards as carbon source, and feed nitrogen simultaneously and under 500 ℃-650 ℃, carry out catalytic cracking reaction; In the mist, V
Nitrogen/ V
Reaction gas=6-12; Mist is 300mL/min-900mL/min by the flow velocity of catalyst; Stop mist after the reaction 1-4h, make stove under nitrogen atmosphere, be chilled to room temperature, obtain CNT and carbon onion.
The weight score of Ni/Al catalyst precursor is meant the nickel aluminium weight ratio in this catalyst precursor.
In a preference of the present invention, in order to obtain better effect, when carrying out catalytic cracking reaction, mist preferably passes through catalyst with the flow velocity of 420mL/min-780mL/min.
The inventive method has following characteristics and advantage:
1) Preparation of Catalyst is simple.
2) output of resulting CNT and carbon onion is big, and reaction back CNT quality is 7-8 a times of catalyst quality, and carbon onion quality is 1.5-2 a times of catalyst quality.
3) quality is good, purity height (more than 90%).Gained CNT caliber less (10-20nm), very even, the tube wall cleaning; Carbon onion particle diameter is also less and very even, the kernel cleaning.
4) be suitable for industrial mass production CNT and carbon onion.
Description of drawings
The TEM figure of the CNT of Fig. 1 the inventive method preparation
The HRTEM figure of the CNT of Fig. 2 the inventive method preparation
The TEM figure of the carbon onion of Fig. 3 the inventive method preparation
The HRTEM figure of the hollow carbon onion of kernel of Fig. 4 the inventive method preparation
The specific embodiment
Further specify the present invention below in conjunction with embodiment, these embodiment only are used to illustrate the present invention, do not limit the present invention.The weight score of Ni/Al catalyst precursor is meant the nickel aluminium weight ratio in this catalyst precursor among the present invention.
The raw material that uses: six water nickel nitrates, commercially available, purity＞96%; Aluminium powder, commercially available, 400 orders.
Get the Ni/Al catalyst precursor of 800mg with the inventive method preparation, after one hour, the weight of products therefrom and increase sees the following form through catalytic cracking reaction.The purity of CNT and carbon onion is respectively up to 96% and 93%, and carbon pipe caliber is at 10-30nm, and length is at 1-15 μ m, and carbon onion particle diameter is at 5-50nm.
| Example number | Ni/Al catalyst precursor weight score/quality (mg) | Dehydration temperaturre (℃) | Calcining heat (℃) | Reduction temperature (℃) | Recovery time (h) | Reaction temperature (℃) | Reaction time (h) | Recovery time VH 2 (mL/min) | Reaction time VN 2/VCH4 (mL/min /mL/min) | The products therefrom composition | Final CNT or carbon onion quality (mg) |
| 1 | 0.025∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | CNT | 800 |
| 2 | 0.052∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | CNT | 3000 |
| 3 | 0.11∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | CNT | 4800 |
| 4 | 0.25∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | CNT | 6400 |
| 5 | 0.67∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | CNT | 7000 |
| 6 | 1.5∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | The carbon onion | 1000 |
| 7 | 4∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 540/60 | The carbon onion | 1500 |
| 8 | 0.25∶1/ 800mg | 240 | 400 | 600 | 2 | 550 | 1 | 100 | 420/60 | CNT | 5000 |
| 9 | 0.25∶1/ 800mg | 240 | 400 | 600 | 2 | 550 | 2 | 100 | 420/60 | CNT | 6000 |
| 10 | 0.25∶1/ 800mg | 240 | 400 | 600 | 2 | 550 | 3 | 100 | 420/60 | CNT | 6500 |
| 11 | 0.25∶1/ 800mg | 240 | 400 | 600 | 2 | 550 | 1 | 100 | 480/60 | CNT | 7200 |
| 12 | 1.5∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 1 | 100 | 420/60 | The carbon onion | 800 |
| 13 | 1.5∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 2 | 100 | 540/60 | The carbon onion | 850 |
| 14 | 1.5∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 3 | 100 | 540/60 | The carbon onion | 1100 |
| 15 | 4∶1/ 800mg | 240 | 400 | 600 | 2 | 600 | 2 | 100 | 540/60 | The carbon onion | 1400 |
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| CNB200510014889XA CN100368080C (en) | 2005-08-29 | 2005-08-29 | Method for preparing carbon nanotubes and carbon onions by Ni/Al catalyst chemical vapor deposition |
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| CNB200510014889XA CN100368080C (en) | 2005-08-29 | 2005-08-29 | Method for preparing carbon nanotubes and carbon onions by Ni/Al catalyst chemical vapor deposition |
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| CN100368080C true CN100368080C (en) | 2008-02-13 |
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Cited By (4)
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| US9862606B1 (en) | 2017-03-27 | 2018-01-09 | Lyten, Inc. | Carbon allotropes |
| CN109147986A (en) * | 2018-09-13 | 2019-01-04 | 慈溪市万金电子元件有限公司 | A kind of carbon onion conductive material of embedded metal and preparation method thereof |
| US10428197B2 (en) | 2017-03-16 | 2019-10-01 | Lyten, Inc. | Carbon and elastomer integration |
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| US10428197B2 (en) | 2017-03-16 | 2019-10-01 | Lyten, Inc. | Carbon and elastomer integration |
| US10920035B2 (en) | 2017-03-16 | 2021-02-16 | Lyten, Inc. | Tuning deformation hysteresis in tires using graphene |
| US11008436B2 (en) | 2017-03-16 | 2021-05-18 | Lyten, Inc. | Carbon and elastomer integration |
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| CN109147986A (en) * | 2018-09-13 | 2019-01-04 | 慈溪市万金电子元件有限公司 | A kind of carbon onion conductive material of embedded metal and preparation method thereof |
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