CN1184141C - Hollow nano carbon ball manufacturing method - Google Patents
Hollow nano carbon ball manufacturing method Download PDFInfo
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- CN1184141C CN1184141C CNB021187304A CN02118730A CN1184141C CN 1184141 C CN1184141 C CN 1184141C CN B021187304 A CNB021187304 A CN B021187304A CN 02118730 A CN02118730 A CN 02118730A CN 1184141 C CN1184141 C CN 1184141C
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- nano carbon
- hollow nano
- carbon microsphere
- manufacture method
- graphite
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- Expired - Lifetime
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- 229910021392 nanocarbon Inorganic materials 0.000 title claims description 69
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 42
- 239000010439 graphite Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000010891 electric arc Methods 0.000 claims abstract description 29
- 238000000746 purification Methods 0.000 claims abstract description 6
- 239000004005 microsphere Substances 0.000 claims description 65
- 239000002041 carbon nanotube Substances 0.000 claims description 40
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 40
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 238000004587 chromatography analysis Methods 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 4
- 229960000800 cetrimonium bromide Drugs 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 3
- 150000001768 cations Chemical group 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 12
- 239000011261 inert gas Substances 0.000 abstract description 2
- 239000002077 nanosphere Substances 0.000 abstract 3
- 239000000047 product Substances 0.000 description 23
- 239000007789 gas Substances 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- -1 alkyl betanidin Chemical compound 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- FPFIFCBPMJFKJR-LLVKDONJSA-M betanidin Natural products O=C([O-])[C+]1/[N+](=C/C=C/2\C=C(C(=O)O)N[C@@H](C(=O)O)C\2)/c2c(cc(O)c(O)c2)C1 FPFIFCBPMJFKJR-LLVKDONJSA-M 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- OKTJSMMVPCPJKN-YPZZEJLDSA-N carbon-10 atom Chemical compound [10C] OKTJSMMVPCPJKN-YPZZEJLDSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002088 nanocapsule Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Images
Abstract
The present invention discloses a method for preparing hollow carbon nano-spheres, which comprises the following steps: (a), an electric arc reaction chamber comprising a graphite anode and a graphite cathode is provided, and inert gas is filled to the electric arc reaction chamber; (b), voltage is applied between the cathode and the anode by pulse current, and therefore, electric arc discharge reactions are generated; (c), products deposited on the graphite cathode are collected. The method is capable of obtaining high-purity hollow carbon nano-spheres (products mainly the hollow carbon nano-spheres), and has the advantages of low cost, easy purification, etc.
Description
Technical field
The present invention relates to the manufacture method of a kind of hollow nano carbon microsphere (hollow carbon nanocapsules), particularly a kind of manufacture method of high purity hollow nano carbon microsphere.
Background technology
The polyhedron carbon that the hollow nano carbon microsphere is made up of with the structure of ball in the ball the multilayer graphite linings bunch, the about 3--60nm of its diameter has special soccerballene (fullerene) structure and photoelectric property, makes it that posture that becomes the rising star be arranged greatly.The hollow nano carbon microsphere can be applicable to many fields, for example: medicine (pharmaceutical grade activated carbon); Light, thermal absorption and electromagnetic shielding; Luminous organic material or solar receiver; Catalyst, transmitter; Carbon dioxide process carbon electrode in the lithium cell; Tool thermal conductance, the multiple material of special electrical nanometer; Printing is with directions such as nano-carbon powders.
Yet, there is no the method for preparing high-purity nano carbon ball in the existing document, only be when making CNT (carbon nano-tube) (nanotubes), to find a small amount of nano carbon microsphere, and quantity enough observation structure under electron microscope only, and because the traditional method products therefrom is to grow CNT (carbon nano-tube), between nano carbon microsphere and carbon pipe strong Fan Dewali is arranged, under the few situation of amount, be difficult for, so that the related application of nano carbon microsphere is limited to standstill state always its separation and purification.
United States Patent (USP) discloses a kind of method of making CNT (carbon nano-tube) and nano particle No. 6063243, and this method mainly is to make CNT (carbon nano-tube), and also obtaining nano particle simultaneously is by product.This patent uses direct current to carry out the arc-over reaction.
German Patent discloses a kind of method of utilizing laser volatilization catalytic process to make nanofiber, nano particle and nano-sized carbon bunch for No. 19740389.This method have manufacturing cost height, productive rate low, can't purifying etc. shortcoming.
Summary of the invention
Main purpose of the present invention provides a kind of manufacture method of hollow nano carbon microsphere, can obtain high purity hollow nano carbon microsphere, is primary product with the hollow nano carbon microsphere.
For reaching above-mentioned purpose, method of the present invention comprises following key step: (a) provide one to contain the electric arc reaction chamber of graphite anode and graphite cathode, and feed a rare gas element in the electric arc reaction chamber; (b) apply a voltage between above-mentioned negative electrode and the anode with a pulsed current, thereby produce the arc-over reaction; And (c) collect the product be deposited on graphite cathode.
In addition, can comprise a purification procedures (d) after step (c), to go out the hollow nano carbon microsphere from above-mentioned product separation and purification, it can comprise: (d1) with an interfacial agent above-mentioned product is scattered in the solution; (d2) separate the principal product and the CNT (carbon nano-tube) of the hollow nano carbon microsphere in the above-mentioned solution with tubing string chromatography or filter membrane; And (d3) separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method.
Specifically, the present invention discloses a kind of manufacture method of hollow nano carbon microsphere, comprises the following steps:
(a) provide one to contain the electric arc reaction chamber of graphite anode and graphite cathode, and in this electric arc reaction chamber, feed a rare gas element;
(b) apply voltage between above-mentioned negative electrode and anode with a pulsed current, thereby produce the arc-over reaction; And
(c) be collected in settling on the graphite cathode.
The flow rate control of described rare gas element is at 30--120cm
3/ min.
The pressure-controlling of described electric arc reaction chamber is at the 1--10 normal atmosphere.
Described graphite anode and graphite cathode are constituted by graphite rod.
The frequency of described pulsed current is 0.01--500Hz.
Described arc-over reaction is carried out under the condition of 10--30 volt and 50--500 ampere with the pulsed current of 0.01--500Hz.
Described step (c) is for collecting the settling of graphite cathode core.
Described settling on graphite cathode comprises the principal product and the CNT (carbon nano-tube) of hollow nano carbon microsphere.
The present invention also discloses a kind of manufacture method of hollow nano carbon microsphere, comprises the following steps:
(a) provide one to contain the electric arc reaction chamber of graphite anode rod and negative electrode graphite rod, and in this electric arc reaction chamber, feed a rare gas element;
(b) apply voltage between above-mentioned negative electrode and anode with a pulsed current, thereby produce the arc-over reaction;
(c) be collected in the settling of negative electrode graphite rod, comprising the principal product and the CNT (carbon nano-tube) of hollow nano carbon microsphere; And
(d) go out the hollow nano carbon microsphere from above-mentioned settling separation and purification.
The flow rate control of described rare gas element is at 30--120cm
3/ min.
The pressure-controlling of described electric arc reaction chamber is at the 1--10 normal atmosphere.
The range of frequency of described pulsed current is 0.01--500Hz.
Described arc-over reaction is carried out under the condition of 10--30 volt and 50--500 ampere with the pulsed current of 0.01--500Hz.
Described step (c) is for collecting the settling of negative electrode graphite rod core.
Described step (d) also comprises:
(d1) with an interfacial agent above-mentioned product is scattered in the solution;
(d2) separate the principal product and the CNT (carbon nano-tube) of the hollow nano carbon microsphere in the above-mentioned solution with the tubing string chromatography; And
(d3) separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method.
Described interfacial agent is cation interfacial active agent, teepol, both sexes interfacial agent or non-ionic interfacial agent.
Described interfacial agent is cetrimonium bromide or sodium lauryl sulphate.
Described step (d2) uses a front end to have the chromatography tubing string of filter membrane.
Described filter membranous layer has the about 0.2 micron hole of size.
The hollow nano carbon microsphere purity of described step (d3) gained is greater than 95%.
Described step (d) also comprises:
(d1) with an interfacial agent above-mentioned product is scattered in the solution;
(d2) separate the principal product and the CNT (carbon nano-tube) of the hollow nano carbon microsphere in the above-mentioned solution with a filter membrane; And
(d3) separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method.
Described filter membrane has the about 0.2 micron hole of size.
For above and other objects of the present invention, feature and advantage can be become apparent, cited below particularlyly go out preferred embodiment, and conjunction with figs., be described in detail below.
Description of drawings
Fig. 1 shows that one is used to implement the synoptic diagram of electric arc reaction of the present invention chamber.
Fig. 2 is electron microscope (TEM) photo of nano carbon microsphere head product.
Fig. 3 is electron microscope (TEM) photo of the nano carbon microsphere behind the purifying.
Fig. 4 is electron microscope (TEM) photo of high nano carbon microsphere of resolving.
Among the figure:
1--electric arc reaction chamber 2--power supply
10--graphite cathode 12--graphite anode
The outlet of 4--inert gas entrance 16--rare gas element
18--cooling water inlet 20--cooling water outlet
Embodiment
Technology of the present invention mainly is under the highly compressed rare gas element (greater than 1 normal atmosphere), utilize pulsed current (pulse current) to carry out the arc-over reaction, the density of electrode surface temperature and carbon vapor when changing arc-over is whereby improved the productivity of carbon ball.
Please refer to Fig. 1, Fig. 1 shows that one is used to implement the synoptic diagram of electric arc reaction of the present invention chamber.In electric arc reaction chamber 1, comprise a pair of electrode 10,12 at least as arc-over.Rare gas element is entered in the electric arc reaction chamber 1 by introducing port 12, is discharged by outlet 16.The periphery of electric arc reaction chamber 1 surrounds with the water coolant that flows, and 16 is the cooling water inlet among the figure, and 18 is cooling water outlet.
In the present invention, electric arc reaction carries out under the mobile rare gas element, and the flow velocity of rare gas element can be controlled in 30--120cm
3/ min, the preferably is controlled at 60--90cm
3/ min.Being applicable to that rare gas element of the present invention comprises is not limited to: helium, argon gas, nitrogen etc.For preparing hollow nano carbon microsphere of the present invention, the pressure of electric arc reaction chamber can be controlled in the 1--10 normal atmosphere, and the preferably can be controlled between the 1--2 normal atmosphere.
In electric arc reaction chamber 1, be provided with two mutual right electrodes 10,12.Electrode 10,12 used herein is all graphite material, generally is as graphite cathode and graphite anode with graphite rod.During preparation hollow nano carbon microsphere, to graphite cathode 10 and graphite anode 12, the electric energy that is provided need make is enough to produce arc-over to form settling on graphite cathode 10 between the two poles of the earth from power supply 2 supply electric energy.
According to principal character of the present invention, when carrying out the arc-over reaction, utilize the pulsed current (pulse current) of a CF to apply a voltage between negative electrode and the anode, be different from used direct current of prior art or alternating-current.According to the present invention, the range of frequency of pulsed current can be between 0.01--500Hz, wherein again with preferable between the 50--70Hz.The controlled amount of electric current is built in the 50--500 ampere, and the voltage between the electrode is controlled at the scope of 10--30 volt approximately.
After carrying out arc-over reaction according to above-mentioned condition, sedimental core can obtain the head product of black powder on negative carbon 10, comprising the principal product (at least greater than 50%) and the short CNT (carbon nano-tube) of hollow nano carbon microsphere.This head product can obtain highly purified hollow nano carbon microsphere through after being further purified.At first, being used in an interfacial agent is scattered in head product in one solution; Then, last with hollow nano carbon microsphere and the CNT (carbon nano-tube) in tubing string chromatography or the filter membrane separation solution, separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method, can obtain purity greater than 95% hollow nano carbon microsphere.
Be applicable to that interfacial agent of the present invention can be cation interfacial active agent, as cetrimonium bromide (certyltrimethyl ammonium bromide), teepol, as sodium lauryl sulphate (sodium dodecyl sulfate), both sexes interfacial agent, as alkyl betanidin (alkyl betaine) or non-ionic interfacial agent, as lauryl alcohol (laurylalcohol ether).Wherein the preferably is cetrimonium bromide and sodium lauryl sulphate.The above-mentioned filtration unit that is used for carrying out the tubing string chromatography can utilize the chromatography tubing string with size exclusion (sizeexclusion) function, and the front end of this chromatography tubing string is preferable to have the about 0.2 micron filter membranous layer in an aperture.In addition, also can use filter membrane to separate separately, and not use the tubing string chromatography.When using filter membrane to separate, filtrate heavily can be filtered for several times in the hope of obtaining preferable separating effect.
Compare with existing technology, the present invention has the following advantages at least:
1. the present invention can obtain highly purified hollow nano carbon microsphere (is principal product with the hollow nano carbon microsphere) method.
2. utilize head product of the present invention to be mainly the short CNT (carbon nano-tube) of about 70% nano carbon microsphere and about 30%, owing to wherein be not difficult for the long CNT (carbon nano-tube) of dispersive, therefore product can be scattered in the liquid phase easily, can utilize in addition purifying of simple and easy, nondestructive method, and be easy to development and use.
3. prepare nano carbon microsphere with method of the present invention, have the advantage that ratio nano carbon pipe manufacturer cost is low, be easy to purifying, can be used to replace CNT (carbon nano-tube).
Present embodiment utilization electric arc reaction chamber as shown in Figure 1 prepares the hollow nano carbon microsphere, and wherein two graphite rods are respectively negative electrode and anode (the graphite rod diameter is 0.24 inch.Negative electrode is shorter, the about 8--10 centimetre of length).In the electric arc reaction chamber, with 60--90cm
3The flow velocity of/min feeds argon gas, and the pressure of reaction chamber is controlled at 1.2 normal atmosphere approximately.The periphery of electric arc reaction chamber is the mobile water coolant.
With the pulsed current of about 60Hz frequency, about 20 volts with about 100 amperes condition under carry out arc-over (carbon arc) reaction.React after about 30 minutes and stop exoelectrical reaction, on negative carbon, can get settling (the about 3--4 centimetre of settling length; Diameter is approximately identical with graphite rod), the incision settling can obtain the head product of black powder in its core, wherein contain have an appointment 70% nano carbon microsphere and about 30% short CNT (carbon nano-tube), and a spot of carbon granules.Please refer to Fig. 2, be depicted as electron microscope (TEM) photo of nano carbon microsphere head product.
Head product is scattered in the solution by an interfacial agent, and the filter method with the tubing string chromatography separates the hollow nano carbon microsphere in the solution with CNT (carbon nano-tube) again.At last, again interfacial agent is separated with the hollow nano carbon microsphere in ultracentrifugal mode.The result can be purified to the hollow nano carbon microsphere high purity more than 95%.Please refer to Fig. 3, be depicted as electron microscope (TEM) photo of the nano carbon microsphere behind the purifying, Fig. 4 then is electron microscope (TEM) photo of high nano carbon microsphere of resolving.
The present invention with preferred embodiment openly as above; so it is not to be used to limit the present invention, those of ordinary skill in the art, without departing from the spirit and scope of the present invention; when can doing a little change and retouching, so protection scope of the present invention is as the criterion with claim.
Claims (11)
1. the manufacture method of a hollow nano carbon microsphere is characterized in that, described method comprises the following steps:
(a) provide one to contain the electric arc reaction chamber of graphite anode and graphite cathode, and in this electric arc reaction chamber, feed a rare gas element;
(b) apply voltage between above-mentioned negative electrode and anode with a pulsed current, thereby produce the arc-over reaction; And
(c) be collected in settling on the graphite cathode;
Wherein
The flow rate control of this rare gas element is at 30-120cm
3/ min, the pressure-controlling of this electric arc reaction chamber is at the 1-10 normal atmosphere, and the arc-over reaction is the pulsed current with 0.01-500Hz, carries out under the condition of 10-30 volt and 50-500 ampere.
2. the manufacture method of hollow nano carbon microsphere as claimed in claim 1 is characterized in that, described graphite anode and graphite cathode are constituted by graphite rod.
3. the manufacture method of hollow nano carbon microsphere as claimed in claim 1 is characterized in that, described step (c) is for collecting the settling of graphite cathode core.
4. the manufacture method of hollow nano carbon microsphere as claimed in claim 3 is characterized in that, described settling on graphite cathode comprises the principal product and the CNT (carbon nano-tube) of hollow nano carbon microsphere.
5. the manufacture method of a hollow nano carbon microsphere comprises the following steps:
(a) provide one to contain the electric arc reaction chamber of graphite anode rod and negative electrode graphite rod, and in this electric arc reaction chamber, feed a rare gas element;
(b) apply voltage between above-mentioned negative electrode and anode with a pulsed current, thereby produce the arc-over reaction;
(c) be collected in the settling of negative electrode graphite rod, comprising the principal product and the CNT (carbon nano-tube) of hollow nano carbon microsphere; And
(d) go out the hollow nano carbon microsphere from above-mentioned settling separation and purification;
Wherein
The flow rate control of this rare gas element is at 30-120cm
3/ min, the pressure-controlling of this electric arc reaction chamber is at the 1-10 normal atmosphere, and the arc-over reaction is carried out under the condition of 10-30 volt and 50-500 ampere with the pulsed current of 0.01-500Hz.
6. the manufacture method of hollow nano carbon microsphere as claimed in claim 5 is characterized in that, described step (c) is for collecting the settling of negative electrode graphite rod core.
7. the manufacture method of hollow nano carbon microsphere as claimed in claim 5 is characterized in that, described step (d) comprising:
(d1) with an interfacial agent above-mentioned product is scattered in the solution;
(d2) separate the principal product and the CNT (carbon nano-tube) of the hollow nano carbon microsphere in the above-mentioned solution with the tubing string chromatography; And
(d3) separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method;
Wherein
This interfacial agent is cation interfacial active agent, teepol, both sexes interfacial agent or non-ionic interfacial agent, and step (d2) uses a front end to have the chromatography tubing string of filter membrane, and this filter membranous layer has the hole of 0.2 micron of size.
8. the manufacture method of hollow nano carbon microsphere as claimed in claim 7 is characterized in that, described interfacial agent is cetrimonium bromide or sodium lauryl sulphate.
9. the manufacture method of hollow nano carbon microsphere as claimed in claim 7 is characterized in that, the hollow nano carbon microsphere purity of described step (d3) gained is greater than 95%.
10. the manufacture method of hollow nano carbon microsphere as claimed in claim 5 is characterized in that, described step (d) comprising:
(d1) with an interfacial agent above-mentioned product is scattered in the solution;
(d2) separate the principal product and the CNT (carbon nano-tube) of the hollow nano carbon microsphere in the above-mentioned solution with a filter membrane; And
(d3) separate above-mentioned interfacial agent and hollow nano carbon microsphere with the rotating centrifugal method.
11. the manufacture method of hollow nano carbon microsphere as claimed in claim 10 is characterized in that, it is 0.2 micron hole that described filter membrane has size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021187304A CN1184141C (en) | 2002-04-30 | 2002-04-30 | Hollow nano carbon ball manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021187304A CN1184141C (en) | 2002-04-30 | 2002-04-30 | Hollow nano carbon ball manufacturing method |
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|---|---|
| CN1454839A CN1454839A (en) | 2003-11-12 |
| CN1184141C true CN1184141C (en) | 2005-01-12 |
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|---|---|---|---|
| CNB021187304A Expired - Lifetime CN1184141C (en) | 2002-04-30 | 2002-04-30 | Hollow nano carbon ball manufacturing method |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100537411C (en) * | 2004-08-20 | 2009-09-09 | 财团法人工业技术研究院 | Nanometer carbon ball with heteroatom and its preparation method |
| CN100374368C (en) * | 2004-12-24 | 2008-03-12 | 中国科学院兰州化学物理研究所 | Method for preparing Nano carbon balls by using pyrolysis of carbon based network polymer |
| CN100425371C (en) * | 2005-01-19 | 2008-10-15 | 鸿富锦精密工业（深圳）有限公司 | Wear resistant appliance and preparation method thereof |
| CN101029218A (en) * | 2006-03-01 | 2007-09-05 | 财团法人工业技术研究院 | Heat-transferring solution containing heteroatomic nano-carbon ball |
| CN100537422C (en) * | 2006-11-07 | 2009-09-09 | 中国科学院理化技术研究所 | Method for preparing hollow micrometre carbon ball with structured size |
| CN101875490B (en) * | 2009-12-17 | 2012-07-18 | 南京工业大学 | Method for synthesizing carbon micron-spheres |
| CN102583304B (en) * | 2011-12-28 | 2013-07-03 | 太原理工大学 | Method for preparing carbon microsphere by utilizing waste cotton fibre |
| CN113351133A (en) * | 2021-07-05 | 2021-09-07 | 西安交通大学 | Gas-liquid two-phase discharge device for preparing carbon nano material and use method thereof |
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2002
- 2002-04-30 CN CNB021187304A patent/CN1184141C/en not_active Expired - Lifetime
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