CN100453455C - Nano carbon material synthesizing device and method - Google Patents
Nano carbon material synthesizing device and method Download PDFInfo
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- CN100453455C CN100453455C CNB2005100356676A CN200510035667A CN100453455C CN 100453455 C CN100453455 C CN 100453455C CN B2005100356676 A CNB2005100356676 A CN B2005100356676A CN 200510035667 A CN200510035667 A CN 200510035667A CN 100453455 C CN100453455 C CN 100453455C
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Abstract
This invention relates to a device for continuously synthesizing nm carbon materials including a first vacuum cavity, a second and a third vacuum cavities and a loader, in which, said second and third vacuum cavities realize on-off with the first via a valve, the first one contains an anode, an exhaust port and a conductor moving relatively to the first one, said second one includes a pump port and a control device, said third vacuum cavity includes a pump port, said loader includes a tank containing cathode, an electrode hole conducting to the tank and a cathode in the tank, in which, said control device sends said loader in said second vacuum cavity into the first and third vacuum cavities and the conductor can be connected with the cathode via said electrode hole when the loader is placed at a preset position in said vacuum cavity. This invention also provides a synthesizing method for the nm carbon material.
Description
[technical field]
The present invention relates to a kind of nano carbon material synthesizing device and method, especially a kind of device and method that utilizes arc discharge method synthesis of nano carbon material.
[background technology]
Arc discharge method is to use the earliest in the synthesis of nano carbon material technology of (comprising nano-carbon powder, CNT (carbon nano-tube), carbon nano fiber, nano carbon microsphere or its mixture etc.), the high temperature that it utilizes arc-over to produce, with material gasification to be deposited as the method for nano material.Nano carbon material has been applied in various fields at present with its higher physical strength and more excellent chemistry, physical property.
1991, Japanology personnel Sumio Iijima people such as (Iijima) at first utilized the arc discharge method synthesis of carbon nanotube.It utilizes two graphite carbon rods to reach the negative electrode that is oppositely arranged with this anode as anode respectively in a vacuum chamber, and the spacing between anode and the negative electrode can be adjusted; Be added with transition metal (as catalyzer such as Fe, Co, Ni, Fe/Ni, Co/Ni) in this anode graphite carbon-point.During work, vacuum chamber is vacuumized, feed mobile rare gas element (as helium or argon gas etc.) again, and keep stable cavity internal pressure; Because of the cooling performance of negative electrode has very big influence to the quality of CNT (carbon nano-tube), thus pass to water coolant at the male-female interpolar earlier, and then between anode and negative electrode, apply a direct current voltage (about 30～50V).Lentamente the anode graphite carbon-point is moved toward fixed negative electrode graphite carbon rod end with uniform velocity, when enough hour of two electrode distances (approximately less than 1 millimeter), produce stable electric arc between two electrodes, the size of control flame current.Like this, the anode graphite carbon-point most advanced and sophisticated can because of moment the high temperature that produced of arc-over gasify, the carbon material of gasification decomposes generation seven-element carbon ring or five yuan of structures such as carbocyclic ring under inert gas atmosphere, be combined into CNT (carbon nano-tube), and then deposit at negative electrode graphite carbon rod end.After arc-over finishes, vacuum chamber is passed to the taking-up product mutually with atmosphere.By the CNT (carbon nano-tube) of arc discharge method preparation, it does not almost have defective aspect atomic arrangement, so it has more excellent chemical and physical properties.
Prior art has disclosed the another kind of method for preparing nano carbon material-nano carbon microsphere, and it places an anode and negative electrode in the one electric arc reaction vacuum chamber, and feeds a rare gas element in vacuum chamber; Apply voltage between above-mentioned anode and negative electrode with a pulsed current, thereby produce the arc-over reaction; Afterwards, collect the product that contains CNT (carbon nano-tube) and nano carbon microsphere that is deposited on negative electrode.Afterwards, carry out separation and purification to obtain required nano carbon microsphere.
In the above-mentioned prior art, all adopt the single vacuum chamber to carry out the preparation of nano carbon material, each all the need vacuumizes so that it obtains certain vacuum tightness this single vacuum chamber; After treating that arc-over finishes, need this vacuum chamber is communicated with atmosphere in order to taking out the nano carbon material product.Whenever carry out an arc-over and prepare nano carbon material, all need vacuumize vacuum chamber and vacuum chamber are communicated with atmosphere; Yet this operating process is longer, and it is not suitable for continuously, produces in enormous quantities.
In view of this, provide a kind of apparatus for continously production of nano carbon material and method real for necessary.
[summary of the invention]
To a kind of nano carbon material synthesizing device and method be described with specific embodiment below, it can realize the continuous manufacturing of nano carbon material.
For realizing foregoing, a kind of nano carbon material synthesizing device is provided, it comprises:
One first vacuum chamber, it includes anode, venting port, and the electrical conductor that can move with respect to this first vacuum chamber;
One second vacuum chamber, it includes bleeding point, and control device, and this second vacuum chamber is realized logical closing via a valve and this first vacuum chamber;
One the 3rd vacuum chamber, it includes bleeding point, and the 3rd vacuum chamber is realized logical closing via a valve and this first vacuum chamber;
One carrier, it comprises a negative electrode standing groove, the electrode hole that is connected with this negative electrode standing groove, and be positioned at the negative electrode of this negative electrode standing groove, above-mentioned control device can be sent this carrier that is loaded in this second vacuum chamber into this first vacuum chamber and the 3rd vacuum chamber, during a predetermined position, this electrical conductor can pass above-mentioned electrode hole and realize being electrically connected with this negative electrode in this carrier is sent to this first vacuum chamber.
Preferably, described anode has a setting device, in order to regulate the spacing between this anode and the negative electrode.
Preferably, described first vacuum chamber comprises the inlet mouth that is oppositely arranged with this venting port.
Preferably, described carrier also comprises at least one arm configuration that extends in its both sides.
Described control device comprises push rod.
Described anodic material is pure graphite, is added with the graphite composite material of catalyzer, and is added with the graphite composite material of catalyzer or promotor.
Preferably, described catalyzer comprises iron, cobalt, nickel, chromium carbide, lanthanum, yttrium and composition thereof.
Preferably, described promotor comprises sulphur and solid sulfate.
Described negative electrode is a graphite block.
And, a kind of nano carbon material synthetic method is provided, it may further comprise the steps:
One first vacuum chamber is evacuated to a predetermined vacuum level, and it comprises the electrical conductor that can move with respect to this first vacuum chamber;
One carrier is loaded in one second vacuum chamber and to this second vacuum chamber is evacuated to this predetermined vacuum level, this second vacuum chamber is realized logical closing via one first valve and this first vacuum chamber, this carrier comprises a negative electrode standing groove, the electrode hole that is connected with this negative electrode standing groove, and be positioned at the negative electrode of this negative electrode standing groove;
Open this first valve, this carrier is sent into a predetermined position of this first vacuum chamber, above-mentioned electrical conductor is inserted this electrode hole so that this electrical conductor forms with this negative electrode is electrically connected;
Close this first valve, feed a rare gas element to this first vacuum chamber;
Carry out arc-over;
One the 3rd vacuum chamber is evacuated to this predetermined vacuum level, and it realizes logical closing via one second valve and this first vacuum chamber;
One stand-by carrier is loaded in this second vacuum chamber and to this second vacuum chamber is evacuated to this predetermined vacuum level;
After treating that arc-over finishes in this first vacuum chamber, this electrical conductor is separated with this carrier;
Open this first valve and second valve, stand-by carrier is sent into this predetermined position in this first vacuum chamber, the carrier that will finish arc-over simultaneously is pushed out to the 3rd vacuum chamber;
Close this first and second valve, the electrode hole that above-mentioned electrical conductor is inserted this stand-by carrier carries out arc-over next time;
This carrier that arc-over is finished takes out in the 3rd vacuum chamber, to obtain the nano carbon material product.
Preferably, consistent to the flow direction of this first vacuum chamber feeding rare gas element with the sense of current that arc-over produces.
Preferably, provide voltage to apply to this anode and negative electrode by AC power, direct supply or pulsed current.
With respect to prior art, the nano carbon material synthesizing device that the technical program provided, it adopts the setting of three vacuum chambers, and first vacuum chamber is used to carry out arc-over, and second and third vacuum chamber is respectively applied for and loads stand-by carrier and unload the carrier that arc-over finishes; These three vacuum chambers all can vacuumize separately, and second and third vacuum chamber adopts a valve to control logical the closing between itself and first vacuum chamber respectively; The electrical conductor that being provided with of this three vacuum chambers cooperates carrier structure and can move with respect to first vacuum chamber can reduce by first vacuum chamber because of vacuumizing the time of wait, and then can reach the continuous manufacturing of nano carbon material, with the purpose of realization volume production.
[description of drawings]
Fig. 1 is the partial cutaway diagrammatic sketch of first embodiment of the invention nano carbon material synthesizing device.
Fig. 2 is the cut-away view along the hatching line II-II of Fig. 1.
[embodiment]
To be described in further detail the embodiment of the invention below in conjunction with accompanying drawing.
Referring to Fig. 1 and Fig. 2, the nano carbon material synthesizing device 1 that first embodiment of the invention provided, it comprises one first vacuum chamber, 10, one second vacuum chambers 20, the 3rd vacuum chamber 30, and a carrier 14.Second vacuum chamber 20 and first vacuum chamber 10 are realized logical closing via a valve 22; The 3rd vacuum chamber 30 and first vacuum chamber 10 are realized logical closing via a valve 32.
Wherein,, be provided with an anode 12, one inlet mouths 16, one venting ports 18 in first vacuum chamber 10 referring to Fig. 1, and an electrical conductor 140.This inlet mouth 16 is provided with the valve (not shown); This venting port 18 is provided with the valve (not shown), and it can link to each other with a vacuum pump.This electrical conductor 140 can be done moving with respect to first vacuum chamber 10 by a control device 141.Preferably, this inlet mouth 16 is oppositely arranged with this venting port 18; So-called inlet mouth 16 is oppositely arranged with venting port 18 and is meant that the inlet mouth 16 and the position of venting port 18 are arranged so that the air flow line and the arc-over sense of current in first vacuum chamber 10 are consistent, reducing the collision probability of gas (as rare gas elementes such as helium or argon gas) molecules and carbocation in first vacuum chamber 10, and then increase its mean free path (Mean-Free-Path).
The voltage character that the material of anode 12 applies in the time of can be according to arc-over is selected; When selecting for use voltage of alternating current to add at anode 12 and arc-over with between the negative electrode time, its material can be selected pure graphite for use, or is added with the graphite composite material of catalyzer, or is added with the graphite composite material etc. of catalyzer and promotor; When selecting for use a pulsed current to apply voltage between anode 12 and negative electrode 142, or when selecting for use volts DS to add between anode 12 and negative electrode 142, its material can be selected the graphite composite material that is added with catalyzer for use, or is added with graphite composite material of catalyzer and promotor etc.Preferably, this anode 12 has a setting device 121, and this setting device 121 can make anode 12 do near the motion that reaches away from negative electrode 142; Can adjust itself and arc-over spacing by this setting device 121 with negative electrode, and then the processing parameter when optimizing arc-over.
Second vacuum chamber 20 is positioned at a side of first vacuum chamber 10, and it can be isolated by the valve 22 and first vacuum chamber 10.This second vacuum chamber 20 has an independent bleeding point 24, and a control device, as push rod 26.Certainly, this control device also can adopt other structure, and as screw rod, it can be reached the purpose that carrier 14 is sent into a predetermined position in first vacuum chamber and all can.This bleeding point 24 is provided with the valve (not shown), and it can connect a vacuum pump and pump it to a predetermined vacuum level, and the setting of this predetermined vacuum level can be decided according in first vacuum chamber 10 the required vacuum tightness of arc-over taking place.This push rod 26 is used for stand-by carrier is pushed to predetermined position in first vacuum chamber, and the carrier that finishes of arc-over, releases first vacuum chamber 10 by the capable transfer function of stand-by carrier.Described predetermined position is meant that the electrode hole of the stand-by carrier that carries negative electrode is just to quasi-conductor 140.
The 3rd vacuum chamber 30 is positioned at a side relative with second vacuum chamber 20 of first vacuum chamber 10, and they can be by valve 32 and 10 isolation of first vacuum chamber.The 3rd vacuum chamber 30 has an independent bleeding point (not shown), this bleeding point is provided with valve, it can connect a vacuum pump and pump it to a predetermined vacuum level, and the setting of this predetermined vacuum level can be decided according in first vacuum chamber 10 the required vacuum tightness of arc-over taking place.The 3rd vacuum chamber 30 is used to accept to be pushed out the carrier that the arc-over of first vacuum chamber 10 finishes.
To specifically describe the nano carbon material synthetic method that adopts above-mentioned nano carbon material synthesizing device below.
Valve-off 22 and 32 is connected to a vacuum pump with venting port 18, and so that one first vacuum chamber 10 is evacuated to a predetermined vacuum level, the setting of this predetermined vacuum level can be decided according to arc-over processing parameter demand.
One carrier 14 is loaded in second vacuum chamber 20 and to this second vacuum chamber 20 is evacuated to above-mentioned predetermined vacuum level.
Open this valve 22,,, this carrier 14 is sent into the predetermined position of this first vacuum chamber 10 as push rod 26 by a control device.
Close this valve 22, electrical conductor 140 is inserted in the electrode hole 144, be electrically connected so that this electrical conductor 140 forms with negative electrode 142 by the start of control device 141; In first vacuum chamber 10, provide the mobile rare gas element, as helium or argon gas etc.; When promptly feeding rare gas elementes, bled by vacuum pump by venting port 18, to form a mobile rare gas element from inlet mouth 16; Keep stable cavity pressure, this pressure range is preferably 1～10 normal atmosphere; The flow of rare gas element is preferably 30～120cm
3/ min (cubic centimetre per minute).Between anode 12 and electrical conductor 140, provide voltage to produce arc-over; This voltage range is preferably 10～35V, and its voltage can be that the pulsed current of 0.01～500HZ applies by a frequency, also can be by exchanging or direct supply apply.Preferably, anode 12 is moved to adjust the distance between anode 12 and the negative electrode 142 to negative electrode 142 ends lentamente,, and then between the two poles of the earth, produce more stable electric arc with optimization arc-over processing parameter by setting device 121; Preferably, control arc-over generation electric current is in 50～500A.Because of the cooling performance of negative electrode has considerable influence to the quality of nano-sized carbon material, can after passing to water coolant between anode 12 and the negative electrode 142, between anode 12 and electrical conductor 140, apply voltage again.
One stand-by carrier 14 is loaded in this second vacuum chamber 20, and by bleeding point 24 being connected to a vacuum pump so that this second vacuum chamber 20 is evacuated to above-mentioned predetermined vacuum level;
After treating that arc-overs finish in first vacuum chamber 10, by the start of control device 141 electrical conductor 140 is pulled out in this electrode hole 144, the carrier 14 that itself and arc-over are finished separates;
Open this valve 22 and 32, the start by push rod 26 is delivered to the above-mentioned predetermined position of first vacuum chamber 10 with stand-by carrier 14, and the carrier 14 that will finish arc-over simultaneously is pushed out to the 3rd vacuum chamber 30.Before opening valve 32, the 3rd vacuum chamber 30 is connected to a vacuum pump by its bleeding point and is pumped down to above-mentioned predetermined vacuum level.
Close this valve 22 and 32, electrical conductor 140 is sent in the electrode hole 144 of this stand-by carrier 14, negative electrode 142 formation of the stand-by carrier of electrical conductor 140 and this 14 are electrically connected to carry out arc-over next time by the start of control device 141.
This carrier 14 that arc-over is finished takes out in the 3rd vacuum chamber 30, to obtain the nano carbon material product.
Can repeat the aforesaid operations step in the present embodiment, realizing continuous synthesis of nano carbon material, and then reach the purpose of volume production.
In addition, those skilled in the art also can do other variation in spirit of the present invention, as the inert gas flow during arc-over in suitable change first vacuum chamber, arc-over produces size of current, or the designs such as structure of carrier are to be used for the present invention, as long as it does not depart from technique effect of the present invention and all can.The variation that these are done according to spirit of the present invention all should be included within the present invention's scope required for protection.
Claims (12)
1. nano carbon material synthesizing device, it comprises:
One first vacuum chamber, it comprises an anode, a venting port, and an electrical conductor that can move with respect to this first vacuum chamber;
One second vacuum chamber, it comprises one first bleeding point, and a control device, this second vacuum chamber is realized logical closing via one first valve and this first vacuum chamber;
One the 3rd vacuum chamber, it comprises one second bleeding point, the 3rd vacuum chamber is realized logical closing via one second valve and this first vacuum chamber; And
One carrier, it comprises a negative electrode standing groove, one electrode hole that is connected with this negative electrode standing groove, an and negative electrode that is positioned at this negative electrode standing groove, above-mentioned control device can be sent this carrier that is loaded in this second vacuum chamber into this first vacuum chamber and the 3rd vacuum chamber, during a predetermined position, this electrical conductor can pass above-mentioned electrode hole and realize being electrically connected with this negative electrode in this carrier is sent to this first vacuum chamber.
2. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described anode has a setting device, in order to regulate the spacing between this anode and the negative electrode.
3. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described first vacuum chamber comprises an inlet mouth that is oppositely arranged with this venting port.
4. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described carrier comprises at least one arm configuration that extends in its both sides.
5. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described control device comprises push rod.
6. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described anodic material is pure graphite, is added with the graphite composite material of catalyzer, or is added with the graphite composite material of catalyzer and promotor.
7. nano carbon material synthesizing device as claimed in claim 6 is characterized in that described catalyzer comprises iron, cobalt, nickel, chromium carbide, lanthanum, yttrium and composition thereof.
8. nano carbon material synthesizing device as claimed in claim 6 is characterized in that described promotor comprises sulphur and solid sulfate.
9. nano carbon material synthesizing device as claimed in claim 1 is characterized in that described negative electrode is a graphite block.
10. nano carbon material synthetic method, it may further comprise the steps:
One first vacuum chamber is evacuated to a predetermined vacuum level, and it comprises an electrical conductor that can move with respect to this first vacuum chamber;
One carrier is loaded in one second vacuum chamber and to this second vacuum chamber is evacuated to this predetermined vacuum level, this second vacuum chamber is realized logical closing via one first valve and this first vacuum chamber, this carrier comprises a negative electrode standing groove, one electrode hole that is connected with this negative electrode standing groove, and a negative electrode that is positioned at this negative electrode standing groove;
Open this first valve, this carrier is sent into a predetermined position in this first vacuum chamber, above-mentioned electrical conductor is inserted this electrode hole so that this electrical conductor forms with this negative electrode is electrically connected;
Close this first valve, feed a rare gas element to this first vacuum chamber;
Carry out arc-over;
One the 3rd vacuum chamber is evacuated to this predetermined vacuum level, and it realizes logical closing by one second valve and this first vacuum chamber;
One stand-by carrier is loaded in this second vacuum chamber and to this second vacuum chamber is evacuated to this predetermined vacuum level;
After treating that arc-over finishes in this first vacuum chamber, this electrical conductor is separated with this carrier;
Open this first valve and second valve, stand-by carrier is sent into this predetermined position in this first vacuum chamber, the carrier that will finish arc-over simultaneously is pushed out to the 3rd vacuum chamber;
Close this first and second valve, the electrode hole that above-mentioned electrical conductor is inserted this stand-by carrier carries out arc-over next time;
This carrier that arc-over is finished takes out in the 3rd vacuum chamber, to obtain the nano carbon material product.
11. nano carbon material synthetic method as claimed in claim 10 is characterized in that the flow direction that feeds a rare gas element to this first vacuum chamber is consistent with the sense of current that arc-over produces.
12. nano carbon material synthetic method as claimed in claim 10 is characterized in that providing between this anode and negative electrode a voltage to apply by AC power, direct supply or pulsed current.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100356676A CN100453455C (en) | 2005-06-30 | 2005-06-30 | Nano carbon material synthesizing device and method |
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| CNB2005100356676A CN100453455C (en) | 2005-06-30 | 2005-06-30 | Nano carbon material synthesizing device and method |
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| CN1891623A CN1891623A (en) | 2007-01-10 |
| CN100453455C true CN100453455C (en) | 2009-01-21 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6063243A (en) * | 1995-02-14 | 2000-05-16 | The Regents Of The Univeristy Of California | Method for making nanotubes and nanoparticles |
| CN2535398Y (en) * | 2002-01-31 | 2003-02-12 | 西安交通大学 | Electric arc discharge device for preparing carbon nano tube |
| CN1398779A (en) * | 2002-06-26 | 2003-02-26 | 天津大学 | Automatic continuous preparing equipment for carbon structural nano-material |
| JP2004307241A (en) * | 2003-04-04 | 2004-11-04 | Ulvac Japan Ltd | Production method for carbon nanotube |
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2005
- 2005-06-30 CN CNB2005100356676A patent/CN100453455C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6063243A (en) * | 1995-02-14 | 2000-05-16 | The Regents Of The Univeristy Of California | Method for making nanotubes and nanoparticles |
| CN2535398Y (en) * | 2002-01-31 | 2003-02-12 | 西安交通大学 | Electric arc discharge device for preparing carbon nano tube |
| CN1398779A (en) * | 2002-06-26 | 2003-02-26 | 天津大学 | Automatic continuous preparing equipment for carbon structural nano-material |
| JP2004307241A (en) * | 2003-04-04 | 2004-11-04 | Ulvac Japan Ltd | Production method for carbon nanotube |
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| CN1891623A (en) | 2007-01-10 |
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