CN1583554A - Temperature controlled arc method for mass preparing amorphous carbon nanometer tubes - Google Patents
Temperature controlled arc method for mass preparing amorphous carbon nanometer tubes Download PDFInfo
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- CN1583554A CN1583554A CN 200410026178 CN200410026178A CN1583554A CN 1583554 A CN1583554 A CN 1583554A CN 200410026178 CN200410026178 CN 200410026178 CN 200410026178 A CN200410026178 A CN 200410026178A CN 1583554 A CN1583554 A CN 1583554A
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Abstract
A temp-controllable arc process for preparing a lot of non-crystal carbon nanotubes features that the 1-6 comsumable anode rod consisting of high-purity graphite and catalyst (the mixture of Fe, Ni. Mg and co) and installed to a rotary disk and the cathode rod made of high-purity graphite are used to arc discharge in the hydrogen gas or in the gas mixture of hydrogen, helium, nitrogen and argon while the temp is regulated to generate non-crystal carbon nanotubes.
Description
Technical field
The present invention is the technology of preparing of carbon nanotube, particularly provide a kind of in temperature-controlling arc furnace the method for mass production non-crystal carbon nano tube.
Background technology
Carbon nanotube has caused various countries investigators' extensive concern and very big interest in worldwide since the Electronic Speculum expert Iijima (S.Iijima Nature 1991) of quilt Japan in 1991 finds.It is seamless, the hollow tube body that is rolled into by the graphite flake layer that carbon atom forms.Generally can be divided into Single Walled Carbon Nanotube (Single-walled carbon nanotube) and multi-walled carbon nano-tubes (Multi-walled carbonnanotube).
Recently, (Amorphous Carbon Nanotubes ACNTs) has received researchist's concern to armorphous carbon nanotube.Non-crystal carbon nano tube is different with general carbon nanotube, and its tube wall is made up of many carbon familys, is characterized in that short range order and long-range are unordered, and caliber is at 3～60nm.Because the special construction of its tube wall can expect that its performance and Single Walled Carbon Nanotube and multi-walled carbon nano-tubes have very big difference.Therefore, produce a large amount of, highly purified non-crystal carbon nano tube so that carry out Performance Detection and applied research just becomes a new problem.
People such as Wang (Wang WL et al.Electrochemical Society Proceedings.1997) once utilized arc process, in helium, pressure is 500torr, discharging current is～100A, voltage is～27V, adopt the graphite anode and cathode, in negative electrode nuclear, obtain carbon nanotube, also found armorphous carbon nanotube.The traditional arc process of this employing can only obtain the carbon nanotube of minute quantity in negative electrode nuclear, output is extremely low.
People such as Ci (Ci LJ et al.Journal of Crystal Growth 2001; Applied Surface Science2003) uses chemical Vapor deposition process (Chemical Vaporization Deposition, CVD) method, with benzene is carbon source, ferrocene and thiophene are catalyzer, in nitrogen atmosphere, obtain the armorphous carbon nanotube that diameter range is 10～60nm under 1100～1200 ℃.This method of bibliographical information can prepare carbon nanotube in a large number, but does not see the value that it is concrete.Document has also been reported the formation mechanism of non-crystal carbon nano tube; And studied the influence of annealing to non-crystal carbon nano tube storage hydrogen, studies show that hydrogen pressure is 10MP after annealing under 2200 ℃, its hydrogen-storage amount can reach 3.98% under the normal temperature.
People such as Nishino (Nishino H et al.Carbon 2003) adopt the CVD method, are catalyzer with poly-four husband's ethene and four water iron(ic) chloride, and in nitrogen, temperature is 900 ℃, can obtain the black powder product of 0.05g; And it is formed mechanism explain; But they do not provide the influence of reaction parameter to the preparation non-crystal carbon nano tube.
For this reason, the invention method that prepare in a large number the high non-crystal carbon nano tube of high purity to the application of carbon nanotube with study significant.
Summary of the invention
The objective of the invention is to, make full use of applicant's utility model patent (ZL 01240373.3 " CNT (carbon nano-tube) electric arc producer " Liu Yongning, Song Xiaolong), provide a kind of method, can improve output and purity at this electric arc furnace mass production non-crystal carbon nano tube.
The technical solution that realizes above-mentioned purpose is, a kind of temperature control arc process of mass production non-crystal carbon nano tube, its equipment principle as shown in Figure 1, (ZL 01240373.3, and name is called: CNT (carbon nano-tube) electric arc producer referring to Chinese patent for principle in detail; Contriver: Liu Yongning, Song Xiaolong).Adopt the graphite cathode and anode to mix arc-over under the atmosphere at hydrogen or with helium, nitrogen, argon gas, the anode rotating disk is for can install 1～6 consumable anode rod simultaneously, anode bar is by φ 6～12mm, length is that the high purity graphite of 100～200mm is made, φ 3～6mm, the blind hole of dark 50～150mm are bored along axis in the end.Be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 1～8.0at% iron, nickel, magnesium and cobalt dust, and (wherein iron is 0～35%; Nickel is 0～35%; Magnesium is 0～50%; Cobalt is 0～35%).Catalyzer is mixed with Graphite Powder 99, insert the blind hole compacting.Negative electrode is the high purity graphite rod of the long 100～200mm of φ 20mm.Negative electrode is the high purity graphite rod; By regulating temperature controlling system, can make reaction vessel under different temperature, generate non-crystal carbon nano tube.
Characteristics of the present invention are:
(1) in 25 ℃～700 ℃ temperature range, carries out arc-over;
(2) anode is 1～6 combined electrode that high purity graphite is made, and wherein catalyzer is charges 1～8.0at% iron, nickel, magnesium and cobalt;
(3) hydrogen or with the mixed atmosphere of helium, nitrogen, argon gas under container inner wall formed a large amount of, highly purified non-crystal carbon nano tube.
Its concrete steps of producing carbon nanotube are:
(1) install cathode and anode after, close fire door, vacuumize, reach predetermined vacuum tightness 10
-3In the Pa;
(2) charge into one or more shielding gas to predetermined pressure;
(3) open heating unit, make its temperature reach predetermined value by regulating electric current;
(4) open starting the arc electric discharge device, make its discharge by regulating electric current, cathode and anode spacing is 1～2mm, and be 10 minutes discharge time;
(5) etc. water-cooled is opened fire door behind normal temperature, scrapes the settling that container inner wall is answered in negate.
Difference with the prior art of the present invention is: conventional arc method (comprising improved before this arc process) is not controlled the temperature of its preparation container.Because temperature is the important factor that influences made of carbon nanotubes, so that the yielding poorly of conventional arc method.And yet there are no the report arc process prepare non-crystal carbon nano tube, substantially all be to use catalystic pyrolysis.Reaction chamber of the present invention is columniform, and diameter is 300mm, long 400mm, and big reaction vessel is very necessary for a large amount of carbon nanotubes of preparation; The anode rotating disk can be placed six roots of sensation consumable anode rod simultaneously.And this reaction vessel significantly improves the output of non-crystal carbon nano tube and purity owing to can produce non-crystal carbon nano tube under differing temps.
In a word, the present invention adopts temperature-controlling arc furnace to mix under the atmosphere at hydrogen or with helium, nitrogen, argon gas, φ 3～6mm is bored along axis in end at the consumable anode rod, the blind hole of dark 50～150mm, be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 1～8.0at% iron, nickel, magnesium and cobalt dust, and (wherein iron is 0～35%; Nickel is 0～35%; Magnesium is 0～50%; Cobalt is 0～35%), can in one hour, produce 6.5 gram non-crystal carbon nano tubes.This method has characteristics such as the highly purified non-crystal carbon nano tube of mass production, and wide suitability for industrialized production application prospect is arranged.
Description of drawings
Fig. 1 produces the device synoptic diagram of non-crystal carbon nano tube for a large amount of high purities of temperature control arc process.------------------removable negative electrode 7---thermocouple 8---turns anode to electrode feeding system 6 to temperature regulating device 5 to vacuum vessel 4 to vacuum pressure gauge 3 to water-cooling system 2 in symbolic representation among Fig. 1: 1.
Accompanying drawing 2 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 600 ℃.
Accompanying drawing 3 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 25 ℃.
Accompanying drawing 4 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 300 ℃.
Accompanying drawing 5 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 400 ℃.
Accompanying drawing 6 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 500 ℃.
Accompanying drawing 7 is the transmission electron microscope photo of the non-crystal carbon nano tube of production in the time of 700 ℃.
Accompanying drawing 8 is the stereoscan photograph of the non-crystal carbon nano tube of production.
Accompanying drawing 9 is the high-resolution-ration transmission electric-lens photo of the non-crystal carbon nano tube of production.
Accompanying drawing 10 is the X ray diffracting spectrum of the non-crystal carbon nano tube of production.
Accompanying drawing 11 is that temperature is to producing the yield effect of non-crystal carbon nano tube.
Accompanying drawing 12 is the influence of temperature to the tube bank diameter of production non-crystal carbon nano tube.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment that accompanying drawing and contriver provide.
The invention provides a kind of temperature control arc process of mass production non-crystal carbon nano tube, its equipment principle as shown in Figure 1, in detail principle referring to utility model patent (ZL 01240373.3 " CNT (carbon nano-tube) electric arc producer " Liu Yongning, Song Xiaolong).Adopt the graphite cathode and anode to mix arc-over under the atmosphere at hydrogen or with helium, nitrogen, argon gas, the anode rotating disk is for can install 1～6 consumable anode rod simultaneously, the consumable anode rod is by φ 6mm～φ 12mm, length is made for the high purity graphite of 100mm～200mm, φ 3mm～φ 6mm is bored along axis in the end, the blind hole of dark 50mm～150mm, blind hole is used to put the charges of catalyzer and Graphite Powder 99.Catalyzer is that (wherein iron is 0～35% for the mixture of 1～8.0wt% iron, nickel, magnesium and the cobalt dust of charges total amount; Nickel is 0～35%; Magnesium is 0～55%; Cobalt is 0～35%).Catalyzer is mixed with Graphite Powder 99, insert the blind hole compacting; Negative electrode is the high purity graphite rod of the long 100～200mm of φ 20mm.
(1) in 25 ℃～700 ℃ temperature range, carries out arc-over;
(2) consumable anode is the combined electrode of 1～6 filling 1～8.0wt% iron, nickel, magnesium and cobalt catalyst;
(3) open starting the arc electric discharge device, make its discharge by regulating electric current, cathode and anode spacing is 1～2mm, and be 10 minutes discharge time;
(4) mix under the atmosphere at hydrogen or with helium, nitrogen, argon gas, the reaction vessel inwall has generated a large amount of, highly purified non-crystal carbon nano tube.
It below is the specific embodiment that the applicant provides.
Embodiment 1:
Device is as accompanying drawing 1, and principle is referring to Chinese patent ZL 01240373.3 in detail.
1～6 consumable anode rod is installed on the anode rotating disk simultaneously, φ 5mm is bored along axis in end at the consumable anode rod, the blind hole of dark 140mm, be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 5.0wt% iron, nickel, magnesium and cobalt dust, and (wherein iron is 20%; Nickel is 20%; Magnesium is 40%; Cobalt is 20%) charge into 500 torr hydrogen in the reactor, the temperature of the reactor that raises then is up to 600 ℃, and striking current is the 80A direct current, and voltage is 32V, and two interpolars keep the distance of 2mm; Its concrete steps of producing carbon nanotube are:
(1) install cathode and anode after, close fire door, vacuumize, reach predetermined vacuum tightness 10
-3Pa;
(2) charge into hydrogen to predetermined pressure;
(3) open heating unit, make its temperature reach predetermined value by regulating electric current;
(4) open starting the arc electric discharge device, make its discharge by regulating electric current; Be 10 minutes discharge time;
(5) etc. water-cooled is opened fire door behind normal temperature, scrapes the settling that container inner wall is answered in negate.Can obtain non-crystal carbon nano tube 6.5 Grams Per Hours (seeing accompanying drawing 2).
Embodiment 2:
Device and experiment condition are with embodiment 1.Only changing temperature is room temperature.Can obtain non-crystal carbon nano tube 0.05 Grams Per Hour (seeing accompanying drawing 3).
Embodiment 3:
Device and experiment condition are with embodiment 1.
Experiment condition is with embodiment 1, and only changing temperature is 300 ℃.Can obtain non-crystal carbon nano tube 0.54 Grams Per Hour (seeing accompanying drawing 4).
Embodiment 4:
Device and experiment condition are with embodiment 1.Only changing temperature is 400 ℃.Can obtain non-crystal carbon nano tube 2.32 Grams Per Hours (seeing accompanying drawing 5).
Embodiment 5:
Device and experiment condition are with embodiment 1.Only changing temperature is 500 ℃.Can obtain non-crystal carbon nano tube 4.56 Grams Per Hours (seeing accompanying drawing 6).
Embodiment 6:
Device and experiment condition are with embodiment 1.Only changing temperature is 700 ℃.Can obtain non-crystal carbon nano tube 3.8 Grams Per Hours (seeing accompanying drawing 7).
Embodiment 7:
Device is with embodiment 1.
1～6 consumable anode rod is installed on the anode rotating disk simultaneously, is filled the mixture (through ball milling) of graphite and catalyzer (5wt%) powder in this rod, wherein contain iron, nickel, magnesium and cobalt mixed catalyst, iron is 20%; Nickel is 20%; Magnesium is 40%; Cobalt is 20%.Charge into the mixed gas of 500 torr hydrogen and nitrogen in the electric arc furnace, the temperature of controlling electric arc furnace then is 600 ℃, and striking current is the 80A direct current, and voltage is 32V, and two interpolars keep the distance of 2mm, and be 10 minutes discharge time.Can obtain non-crystal carbon nano tube 3 Grams Per Hours.
Embodiment 8:
Device is with embodiment 1.
1～6 consumable anode rod is installed on the anode rotating disk simultaneously, φ 5mm is bored along axis in end at the consumable anode rod, the blind hole of dark 140mm, be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 2.0at% iron, nickel, magnesium and cobalt dust, and (wherein iron is 20%; Nickel is 20%; Magnesium is 40%; Cobalt is 20%) charge into the mixed gas of 500 torr hydrogen and helium in the electric arc furnace, the temperature of controlling electric arc furnace then is 600 ℃, striking current is the 80A direct current, voltage is 32V, two interpolars keep 1.5mm apart from being discharge time 10 minutes.Can obtain non-crystal carbon nano tube 1 Grams Per Hour.
Embodiment 9:
Device is with embodiment 1.
1～6 consumable anode rod is installed on the anode rotating disk simultaneously, φ 5mm is bored along axis in end at the consumable anode rod, the blind hole of dark 140mm, be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 6.0at% iron, nickel, magnesium and cobalt dust, and (wherein iron is 20%; Nickel is 20%; Magnesium is 40%; Cobalt is 20%) charge into 500 torr hydrogen and the mixed gas of argon in the reactor, the temperature of controlling reactor is 600 ℃ then, and striking current is the 80A direct current, and voltage is 32V, and two interpolars keep the distance of 1mm, and be 10 minutes discharge time; Can obtain non-crystal carbon nano tube 1 Grams Per Hour.
Embodiment 10:
Device is with embodiment 1.
1～6 consumable anode rod is installed on the anode rotating disk simultaneously, φ 5mm is bored along axis in end at the consumable anode rod, the blind hole of dark 140mm, be filled with the charges that graphite and catalyzer are formed in the blind hole, wherein catalyzer is the mixture of charges total amount 8.0at% iron, nickel, magnesium and cobalt dust, and (wherein iron is 20%; Nickel is 20%; Magnesium is 40%; Cobalt is 20%) charge into the mixed gas of 500 torr hydrogen, helium, nitrogen and argon in the reactor, the temperature of controlling reactor is 600 ℃ then, and striking current is the 80A direct current, and voltage is 32V, and two interpolars keep the distance of 2mm, and be 10 minutes discharge time; Can obtain non-crystal carbon nano tube 2 Grams Per Hours.
Claims (4)
1. method that adopts temperature-controlling arc furnace mass production non-crystal carbon nano tube, use temperature control electric arc producer, the characteristics of this equipment are that the temperature that a heating unit is controlled the stainless steel reaction internal tank is installed outside the carbon nanotube reaction vessel, temperature outreaches the temperature dial plate with thermocouple, comes the controlled temperature scope at 25 ℃～900 ℃ by the size of regulating electric current; Reaction vessel interior has anode rotating disk and the negative electrode that 1～6 consumable anode rod is installed simultaneously; Adopt the graphite cathode and anode to mix arc-over under the atmosphere at hydrogen or with helium, nitrogen, argon gas; It is characterized in that consumable anode rod is made for high purity graphite, the end is drilled with blind hole along axis, is filled with Graphite Powder 99 and catalyzer in the blind hole, and wherein catalyzer is 1～8.0% iron, nickel, magnesium and a cobalt dust mixture of charges total amount; Negative electrode is the high purity graphite rod; By regulating the temperature controlling system of carbon nanotube electric arc producer, make the carbon nanotube reaction vessel in 25 ℃～700 ℃ temperature range, carry out arc-over, mix under the atmosphere at hydrogen or with helium, nitrogen, argon gas, carbon nanotube reaction vessel inwall generates highly purified amorphous carbon nanotube.
2. the method for employing temperature-controlling arc furnace mass production non-crystal carbon nano tube as claimed in claim 1 is characterized in that, the concrete steps of producing carbon nanotube are:
(1) install cathode and anode after, close fire door, vacuumize, reach predetermined vacuum tightness 10
-3In the Pa;
(2) charge into hydrogen or with helium, nitrogen, argon gas hybrid protection gas to predetermined pressure;
(3) open heating unit, make its temperature reach predetermined value by regulating electric current;
(4) open starting the arc electric discharge device, make its discharge by regulating electric current, cathode and anode spacing is 1～2mm, and be 10 minutes discharge time;
(5) etc. water-cooled is opened fire door behind normal temperature, scrapes the settling that container inner wall is answered in negate.
3. according to the method for the described employing temperature-controlling arc furnace of claim 1 mass production non-crystal carbon nano tube, it is characterized in that: described blind hole is φ 6mm～φ 12mm, and long is 100mm～200mm.
4. according to the method for the described employing temperature-controlling arc furnace of claim 1 mass production non-crystal carbon nano tube, it is characterized in that: the iron of described 1～8.0wt%, nickel, magnesium and cobalt dust mixture, wherein iron is 0～35%; Nickel is 0～35%; Magnesium is 0～50%; Cobalt is 0～35%.
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| CN 200410026178 CN1261350C (en) | 2004-05-27 | 2004-05-27 | Temperature controlled arc method for mass preparing amorphous carbon nanometer tubes |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351174C (en) * | 2005-12-12 | 2007-11-28 | 西安交通大学 | Method for producing fullerene by temperature-controlling arc furnace |
| CN102001644A (en) * | 2010-12-16 | 2011-04-06 | 中国科学院高能物理研究所 | Automatic packing type electric arc synthetic furnace |
| CN102161480A (en) * | 2010-12-16 | 2011-08-24 | 中国科学院高能物理研究所 | Carbon nano-material automatic synthesis equipment, and control device and control method thereof |
| CN102502586A (en) * | 2011-11-08 | 2012-06-20 | 天津大学 | Method for directly growing amorphous carbon nano tube on iron-based amorphous powder |
-
2004
- 2004-05-27 CN CN 200410026178 patent/CN1261350C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351174C (en) * | 2005-12-12 | 2007-11-28 | 西安交通大学 | Method for producing fullerene by temperature-controlling arc furnace |
| CN102001644A (en) * | 2010-12-16 | 2011-04-06 | 中国科学院高能物理研究所 | Automatic packing type electric arc synthetic furnace |
| CN102161480A (en) * | 2010-12-16 | 2011-08-24 | 中国科学院高能物理研究所 | Carbon nano-material automatic synthesis equipment, and control device and control method thereof |
| CN102001644B (en) * | 2010-12-16 | 2012-08-29 | 中国科学院高能物理研究所 | Automatic packing type electric arc synthetic furnace |
| CN102161480B (en) * | 2010-12-16 | 2012-11-21 | 中国科学院高能物理研究所 | Carbon nano-material automatic synthesis equipment, and control device and control method thereof |
| CN102502586A (en) * | 2011-11-08 | 2012-06-20 | 天津大学 | Method for directly growing amorphous carbon nano tube on iron-based amorphous powder |
| CN102502586B (en) * | 2011-11-08 | 2013-07-24 | 天津大学 | Method for directly growing amorphous carbon nano tube on iron-based amorphous powder |
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