CN100369808C - Method for preparing carbon rod of containing catalyst and sintering unit - Google Patents
Method for preparing carbon rod of containing catalyst and sintering unit Download PDFInfo
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- CN100369808C CN100369808C CNB2004100918518A CN200410091851A CN100369808C CN 100369808 C CN100369808 C CN 100369808C CN B2004100918518 A CNB2004100918518 A CN B2004100918518A CN 200410091851 A CN200410091851 A CN 200410091851A CN 100369808 C CN100369808 C CN 100369808C
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- carbon
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Abstract
The present invention relates to a method for producing a carbon rod containing a catalyst and a sintering device thereof. The sintering device comprises two half molds and a pressing device, wherein the half molds can be matched with each other to form a mold cavity of which one end is closed and the other end is opened, and the pressing device can extend into the mold cavity and is matched with the two half molds. The present invention also provides the method which utilizes the sintering device to produce a carbon rod containing a catalyst, wherein the carbon rod on which catalyst particles are evenly distributed can be produced by the powder sintering technology.
Description
[technical field]
The present invention relates to a kind of preparation method and its agglomerating plant that contains the carbon-point of catalyzer.
[background technology]
Carbon nanotube is the hollow carbon pipe of finding first in by the product of Iijima at arc-over in 1991, and it is published in the Nature354 that publishes in 1991,56.Carbon nanotube is with its good conductivity, perfect crystalline network, characteristics such as the tip of nanoscale and become the filed emission cathode material that has hope have wide prospect in Application Areass such as field emission planar display device, electron tube, HIGH-POWERED MICROWAVES devices.
The preparation method of carbon nanotube mainly comprises pulse laser method of evaporation, chemical Vapor deposition process and arc discharge method.The pulsed laser method of evaporation is to utilize the high-energy of pulsed laser to evaporate the graphite target acquisition carbon nanotube that contains metal catalyst; Chemical Vapor deposition process be with the transition metal of nanoscale or its oxide compound as catalyzer, the carbonaceous source of pyrolysis gas prepares carbon nanotube under low relatively temperature; Arc discharge method is the Graphite Electrodes arc-over acquisition carbon nanotube that utilizes pure graphite or be mixed with metal catalyst.
The advantage of using arc discharge method to prepare carbon nanotube is to prepare carbon nanotube in a large number.Its general preparation process is: vacuumize the back and feed shielding gas; the power supply that activate to connect Graphite Electrodes makes the anode tip temperature reach 4000 ℃ and arc-over takes place; an anodic top part is evaporated vaporization; a large amount of active carbon particles and carbon neutral particle produce and enter arc discharge area; repeat between the particle to bump and further generate carbon ion and active carbon particle; and on anode, negative electrode and arc discharging device inwall, depositing one deck cigarette ash, it comprises carbon nanotube or soccerballene etc.When graphite anode included the metal catalyst particle, Single Walled Carbon Nanotube can generate in a large number.
At present, the anode of arc discharge method, negative electrode all are the carbon-point structure, and this carbon-point can be divided into graphite carbon rod, amorphous carbon-point and active carbon-point by the carbon material difference.In order to increase carbon nanotube output, but carbon-point doping metals catalyst particle, and it mainly adopts following dual mode to be realized: (1) applies or deposition layer of metal catalyst particle at carbon-point one end surfaces; (2) in the middle of carbon-point, imbed a spill.But the carbon-point of making by aforesaid method has that metallics consumes easily and shortcoming pockety in carbon-point.
In view of this, provide a kind of method and its equipment for preparing the carbon-point that evenly is doped with catalyzer to be necessity in fact.
[summary of the invention]
The object of the present invention is to provide a kind of agglomerating plant that contains the carbon-point of catalyzer.
Another object of the present invention is to provide a kind of uses above-mentioned agglomerating plant preparation to contain the method for the carbon-point of catalyzer.
For realizing the object of the invention, the invention provides a kind of agglomerating plant that contains the carbon-point of catalyzer, it comprises:
A two-half die and a hold-down gear;
This two-half die can cooperate formation one die cavity, the sealing of one end, the other end opening;
This hold-down gear can stretch into this die cavity, and cooperates with this two-half die.
For realizing another purpose of the present invention, the invention provides a kind of method of using above-mentioned agglomerating plant to prepare the carbon-point that contains catalyzer, it comprises step:
Prepare carbon dust and catalyst particle and it is mixed the formation mixture;
Combination two-half die formation one has the mould of die cavity, the sealing of one end, the other end opening;
In the opening end injection die cavity of mixture that makes by mould;
Use hold-down gear to exert pressure, make the closely pressing of mix powder quilt in the die cavity to die cavity;
Above-mentioned mould of sintering and hold-down gear;
Cooling die also carries out the demoulding.
Compared with prior art, use agglomerating plant of the present invention to prepare the method for the carbon-point that contains catalyzer owing to adopt powder sintered mode to make carbon electrode, catalyst particle is evenly distributed in the carbon-point, catalyst particle is not easy to consume in the preparation carbon nanotube process, and the carbon nanotube product of preparation is preferable.
[description of drawings]
Fig. 1 is the decomposing schematic representation of agglomerating plant of the present invention.
Fig. 2 is the combination synoptic diagram of agglomerating plant of the present invention.
[embodiment]
The present invention prepares homodisperse has the method for the carbon-point of catalyst particle mainly to adopt sintered powder technique.Sintered powder technique is that catalyst metal powder and carbon dust are squeezed in the mould of specified shape, the mixed powder that this is loose is squeezed into powder, the powder that this is pressed is sent into High Temperature Furnaces Heating Apparatus internal heating sintering then, make powder each other bond form the carbon-point product together.
The invention provides a kind of agglomerating plant that contains the carbon-point of catalyzer, it comprises: a two-half die and a hold-down gear; This two-half die can cooperate formation one die cavity, the sealing of one end, the other end opening; This hold-down gear can stretch into this die cavity, and cooperates with this two-half die.
The present invention is described in further detail below in conjunction with drawings and Examples.
See also Fig. 1, the agglomerating plant of present embodiment, it comprises: two-phase is with the half module 12,12 of shape size ' and pressure rod 14.This two-half die 12,12 ' and pressure rod 14 by can resistant to elevated temperatures die steel or wolfram varbide make.
This two-half die 12,12 ' all be six cubess of strip, it respectively comprises a molding surface 122 and the buckling surface 124 relative with this molding surface.
This two-half die 12,12 ' at these molding surface 122 centers is provided with half-cylindrical die cavity 1221 along its length, and the size of this die cavity 1221 can design according to prepared carbon-point size, and certainly, this die cavity 1221 also can design arbitrarily according to made carbon-point shape.
Be provided with the diameter tail end groove 1223 bigger at the blind end of this die cavity 1221, be used to place the baffle plate (figure does not show) that adds than die cavity 1221.Be provided with two engaging groove 1225 at the other end of die cavity 1221, this engaging groove 1225 is with suitable distance interval, and its diameter is bigger slightly than die cavity 1221.Present embodiment tail end groove 1223 and the design that adds baffle plate (figure do not show) can be born punching press and seepage pressurized powder, conveniently stripped between two-half die not, and can evade die steel or the more unmanageable shortcoming of wolfram varbide.
The locking latches of this buckling surface 124 is a plurality of locked mode grooves 1241 and a plurality of C type clasp (figure does not show) with simple structure.These a plurality of locked mode grooves 1241 are located at the place, two long limits of buckling surface 124, and a plurality of C type clasps (figure does not show) fasten two-half die 12,12 ' corresponding locked mode groove 1241, be used to lock two- half die 12,12 '.Under the requirement of satisfying the locking mould, can design the quantity of locked mode groove 1241 arbitrarily.Present embodiment respectively is provided with the locked mode groove 1241 of three same intervals along two long limits, wherein, two locked mode grooves 1241 are near these half module 12 two ends.
The die cavity shape unanimity that this pressure rod 14 roughly forms with two-half die 12,12 ' fastening back.The pressure rod 14 that this enforcement is adopted comprises that first flange 141, second flange 145 and that are located at two ends are located at 143: the first flanges 141 of tapered protrusion and these die cavity 1221 equal diameters between these two ends, head into die cavity 1221 when being used to pressurize; The bottom surface diameter of this tapered protrusion 143 is than these die cavity 1221 slightly larger in diameter, and its conical surface is towards first flange 141, is used for and engages groove 1225 and be interlocked; With second flange 145 is one to have larger-diameter cylinder shape projection, is used for convenient pressurization, and it can directly be exerted pressure by oil press or mallet.First flange 141 and second flange 145 that are appreciated that the pressure rod 14 of present embodiment are not the parts of necessity of the present invention, this pressure rod 14 also can be the bar that a diameter is less than or equal to this die cavity 1221, be provided with tapered protrusion between its two ends, its diameter is bigger slightly than this die cavity diameter.This pressure rod structure also can realize the pressurization function of agglomerating plant of the present invention.
When the agglomerating plant of present embodiment uses, need two-half die 12,12 ' make up (as shown in Figure 2) at first, is placed the baffle plate (figure does not show) of an appropriate size at the tail end groove 1223 of half module 12; With another identical half module 12 ' tail end groove (indicate) also insert this baffle plate, make this two-half die 12,12 ' molding surface staggered relatively; This two-half die 12,12 ' the relative a plurality of locked mode grooves 1241 of buckling surface on by a plurality of C type clasps (figure does not show) closely fasten this two-half die 12,12 '; Toward two-half die 12, inject the mixture of carbon dust and granules of catalyst in the die cavity of 12 ' formation, then, pressurize by pressure rod 14, first flange 141 of pressure rod 14 enters die cavity 1221 under pressurized, enter engaging groove 1225 and blocked by it in appropriate location tapered protrusion 143, the design of wherein a plurality of engaging grooves 1225 is required for adapting to different powdered mixture amounts; At last above-mentioned mould and pressure rod are put into High Temperature Furnaces Heating Apparatus and carry out sintering.
Be understandable that, agglomerating plant of the present invention is satisfying catalyst fines and carbon dust is squeezed in the mould with specified shape die cavity and mixed powder is squeezed under the requirement of powder, and those skilled in the art can carry out appropriate change to the mould of the foregoing description:
As for two-half die, can be designed to difform two-half die with mutual fastening function, as long as it cooperatively interacts and can form die cavity, form die cavity as a half module, another half module is the plane locked die.And the cavity closed end also can be provided with up and down two-half die and directly cooperates and form the structure that an end seals the die cavity of an end opening, and its fit system can be engaging, fastening, anchor closes or screw togather etc.In addition, to the locking latches of two-half die also can be provided with convenient two-half die engaging, fastening up and down in the molding surface of two-half die, anchor closes or the structure that screws togather, perhaps adopts dismountable modes such as adding the binding two-half die that two-half die is locked.
As for pressure rod, can change into and adopt compressing structure with spiral locking function, cooperate corresponding with it, two-half die can form internal thread at the die cavity of opening end, and this spiral compressing structure forms outside screw.Or directly employing can be stretched into the compressing structure of die cavity, fixes by modes such as outside anchor close at last, as long as it can compress the mixed powder in the die cavity.
Those skilled in the art also can do other variation in spirit of the present invention, certainly, the variation that these are done according to spirit of the present invention, all should be included in the present invention's scope required for protection in.
The present invention uses above-mentioned agglomerating plant preparation to contain the method for the carbon-point of catalyzer, and it comprises step:
(1) preparation carbon dust and catalyst particle and it is mixed, this carbon dust can be selected Graphite Powder 99, amorphous carbon powder and activated carbon powder for use, and this catalyst particle can be selected iron, cobalt, nickel and its alloy for use.
(2) combination two-half die formation one has the mould of die cavity.Agglomerating plant according to the foregoing description can be placed a baffle plate at the tail end groove of two-half die, and fasten this two halves module and become to have the full die of die cavity, mould one end opening, the other end is by this baffle plate sealing, then, closely fasten this two-half die by a plurality of C type clasps.Certainly, the combination of the two-half die of other structure can be closed by engaging, fastening, anchor or screw-in version is fited this two-half die according to practical situation, locks this two-half die by a locking latches again, makes the two halves module become a full die.
(3) mixture that step (1) is made is injected in the die cavity by opening end.
(4) use hold-down gear to exert pressure, make the closely pressing of mix powder quilt in the die cavity to die cavity.First flange of pressure rod can be aimed at the opening end of this mould according to the foregoing description, exert pressure to second flange by oil press or mallet, in pressure process, the tapered protrusion of pressure rod enters die cavity and is blocked by a plurality of engaging grooves, and mix powder is by closely pressing.
(5) mould and the hold-down gear that will press mix powder put into High Temperature Furnaces Heating Apparatus, carries out sintering, make powder each other bond form the carbon-point product together.
(6) cooling die and carry out the demoulding.
Agglomerating plant of the present invention has following several advantages: one, this agglomerating plant is simple in structure to be easy to Processing, because of the mold materials of powder metallurgy, as: tungsten carbide, mould steel etc. all is difficult for processing, so design Simple die shape can conveniently utilize the discharge processing mode to make; Its two, be easy to the demoulding behind the sintering, only Need but C type clasp is knocked out just die sinking, needn't worry to use the screw locked mode, because thermal deformation can't the demoulding Problem.
Use agglomerating plant of the present invention to prepare the method for the carbon-point that contains catalyst owing to adopt powder sintered Mode make carbon electrode, catalyst particle is uniformly distributed in the carbon-point, preparation CNT mistake Catalyst particle is not easy to consume in the journey, and the carbon nanotube product of preparation is better.
Claims (17)
1. agglomerating plant that contains the carbon-point of catalyzer, it comprises:
A two-half die and a hold-down gear;
This two-half die cooperates formation one die cavity, the sealing of one end, the other end opening;
This hold-down gear stretches into this die cavity, and cooperates with this two-half die.
2. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 1, it is characterized in that this two-half die structure is identical, it comprises a molding surface and the buckling surface relative with this molding surface, this buckling surface is provided with a locking latches along the limit, this molding surface is provided with a die cavity along its length, this die cavity one end sealing, the other end of this die cavity are provided with an engaging groove.
3. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 1 is characterized in that this hold-down gear is a pressure rod, and it comprises the tapered protrusion of being located between the two ends, and its diameter is bigger slightly than this die cavity diameter.
4. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 1 or 2 is characterized in that this two-half die made by die steel or tungsten carbide material.
5. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 3 is characterized in that this pressure rod made by die steel or tungsten carbide material.
6. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 2 is characterized in that this locking latches comprises a plurality of locked mode groove and a plurality of C type clasps of being located at these buckling surface two long limits.
7. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 2, the die cavity that it is characterized in that this half module is for half-cylindrical.
8. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 2 is characterized in that the diameter of this engaging groove is bigger than this die cavity.
9. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 2 is characterized in that the blind end of this die cavity is provided with the diameter groove bigger than this die cavity, and it is used to place the baffle plate that adds.
10. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 3 is characterized in that the two ends of this pressure rod are respectively equipped with one first flange and one second flange.
11. the agglomerating plant that contains the carbon-point of catalyzer as claimed in claim 10 is characterized in that the diameter of this first flange is less than or equal to this die cavity diameter, this second lip diameter is greater than the diameter of first flange.
12. a method for preparing the carbon-point that contains catalyzer, it comprises step:
Prepare carbon dust and catalyst particle and it is mixed the formation mixture;
Combination two-half die formation one has the mould of die cavity, the sealing of one end, the other end opening;
In the opening end injection die cavity of mixture that makes by mould;
Use hold-down gear to exert pressure, make the closely pressing of mix powder quilt in the die cavity to die cavity;
Above-mentioned mould of sintering and hold-down gear;
Cooling die also carries out the demoulding.
13. preparation as claimed in claim 12 contains the method for catalyzer carbon-point, it is characterized in that this carbon dust comprises Graphite Powder 99, amorphous carbon powder and activated carbon powder.
14. preparation as claimed in claim 12 contains the method for catalyzer carbon-point, it is characterized in that this this catalyst particle comprises iron, cobalt, nickel and its alloy.
15. preparation as claimed in claim 12 contains the method for catalyzer carbon-point, the combination that it is characterized in that this two-half die is closed by engaging, fastening, anchor or screw-in version is fited this two-half die, lock this two-half die by a locking latches again, make the two halves module become a full die.
16. preparation as claimed in claim 12 contains the method for catalyzer carbon-point, it is characterized in that this hold-down gear is a pressure rod, it comprises the tapered protrusion of being located between the two ends, and its diameter is bigger slightly than this die cavity diameter, and the die cavity that is used for forming with two-half die matches.
17. preparation as claimed in claim 16 contains the method for catalyzer carbon-point, it is characterized in that pressurizeing to this pressure rod by oil press or mallet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100918518A CN100369808C (en) | 2004-12-24 | 2004-12-24 | Method for preparing carbon rod of containing catalyst and sintering unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100918518A CN100369808C (en) | 2004-12-24 | 2004-12-24 | Method for preparing carbon rod of containing catalyst and sintering unit |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1796274A CN1796274A (en) | 2006-07-05 |
| CN100369808C true CN100369808C (en) | 2008-02-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2004100918518A Expired - Fee Related CN100369808C (en) | 2004-12-24 | 2004-12-24 | Method for preparing carbon rod of containing catalyst and sintering unit |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103934400A (en) * | 2014-03-17 | 2014-07-23 | 天津机辆轨道交通装备有限责任公司 | Pull rod forging tool of expanding device |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59123165A (en) * | 1982-12-28 | 1984-07-16 | Matsushita Electric Ind Co Ltd | Manufacture of nonburning carbon rod |
| CN86207121U (en) * | 1986-09-29 | 1987-08-19 | 王振声 | Crayon fabricating apparatus |
| CN1130163A (en) * | 1995-02-26 | 1996-09-04 | 薛天瑞 | Method for directly quick-sintered silicone-carbon stick |
| CN1144787A (en) * | 1995-02-16 | 1997-03-12 | 薛天瑞 | One-step burning method for silicon-carbon bar cold-extruded formed belt end |
| JP2003054922A (en) * | 2001-08-13 | 2003-02-26 | Sony Corp | Structure including carbon-coated catalyst nanoparticle, method of making such structure, and method of producing carbon nanostructure therefrom |
-
2004
- 2004-12-24 CN CNB2004100918518A patent/CN100369808C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59123165A (en) * | 1982-12-28 | 1984-07-16 | Matsushita Electric Ind Co Ltd | Manufacture of nonburning carbon rod |
| CN86207121U (en) * | 1986-09-29 | 1987-08-19 | 王振声 | Crayon fabricating apparatus |
| CN1144787A (en) * | 1995-02-16 | 1997-03-12 | 薛天瑞 | One-step burning method for silicon-carbon bar cold-extruded formed belt end |
| CN1130163A (en) * | 1995-02-26 | 1996-09-04 | 薛天瑞 | Method for directly quick-sintered silicone-carbon stick |
| JP2003054922A (en) * | 2001-08-13 | 2003-02-26 | Sony Corp | Structure including carbon-coated catalyst nanoparticle, method of making such structure, and method of producing carbon nanostructure therefrom |
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| CN1796274A (en) | 2006-07-05 |
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