CN104451960A - Preparation method of carbon microtree - Google Patents
Preparation method of carbon microtree Download PDFInfo
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- CN104451960A CN104451960A CN201410666985.1A CN201410666985A CN104451960A CN 104451960 A CN104451960 A CN 104451960A CN 201410666985 A CN201410666985 A CN 201410666985A CN 104451960 A CN104451960 A CN 104451960A
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Abstract
The invention discloses a method for preparing carbon microtree by utilizing chemical vapor deposition. The method comprises the following steps: introducing a carbon source gas into a deposition chamber from the bottom of a vertical heating furnace and depositing and growing the carbon microtree in an 850-1000DEG C constant-temperature space by utilizing hydrogen as a carrier gas according to the ratio of the carbon source gas to hydrogen being 1:(3-8), wherein the deposition chamber is a cylindrical graphite piece, and a matrix is placed on the inner wall of a graphite cylinder; a device for adsorbing carbon black is hung at the center of the deposition chamber, the device for adsorbing carbon black is a graphite rod with the diameter which is 15-25% that of an effective constant-temperature zone, and the height which is 60-80% that of the effective constant-temperature zone, and the carbon microtree with the diameter of 50-200macrometers and the length of 0.5-1.5millimeters is prepared. A catalyst is not introduced, and thus the growing carbon microtree is high in purity, good in quality, and has good application prospects in the fields of medicals, biology and molecular electronics.
Description
affiliated field
The present invention relates to the preparation method of the micro-tree of a kind of chemical vapour deposition (CVD) charcoal.
technical background
The micro-tree of charcoal is the one of carbon fiber, owing to self having high slight, low-density, excellent thermal conductivity and electric conductivity, is widely used in biomedical and field of molecular electronics.But the micro-tree of charcoal prepared by conventional method needs to introduce metallic catalyst usually, and the catalyst in the micro-tree of charcoal often cannot thoroughly be removed.Biomedical and molectronics often needs the micro-tree of high-quality charcoal, and wherein most important standard is exactly purity and the uniformity of the micro-tree of charcoal.Introduce the technical bottleneck that the high micro-tree material of charcoal of the good purity of manufacture uniformity becomes association area.
summary of the invention
The object of the invention is to utilize chemical vapour deposition (CVD) under the condition not introducing catalyst, the micro-tree of uniform charcoal is prepared in growth, effectively achieves the optimization of the micro-tree construction of charcoal and performance.
The present invention realizes goal of the invention by the following method:
One, to prepare preparation method for the purpose of the micro-tree of the uniform charcoal of high-purity, utilizes carbon-source gas and carrier gas (hydrogen), on different substrates in the 850-1000 ° of micro-tree of C deposition growing charcoal, is 1:(3 ~ 8 by controlling the ratio of carbon-source gas and hydrogen).Substrate is positioned on the inwall of graphite tube (settling chamber).Be positioned at the position of central authorities of settling chamber, be provided with carbon black adsorbent equipment, the diameter of carbon black adsorbent equipment is the 15-25% of diameter between effective flat-temperature zone, and length is the 60-80% of height between effective flat-temperature zone.
Described carbon black adsorbent equipment is the graphite rod of absorption carbon black.
Described carbon-source gas is propylene, natural gas or methane etc.
Described settling chamber is the graphite piece of tubular, and matrix is placed on the inwall of graphite tube.
Described substrate is smooth pyrolytic carbon, pyrolytic graphite, graphite paper or isostatic pressing formed graphite substrate, wherein pyrolytic carbon and pyrolytic graphite can be deposited on graphite tube inwall as substrate, graphite paper can be attached to graphite tube inwall as substrate, and isostatic pressing formed graphite can directly be processed into graphite tube as substrate.
The present invention does not introduce catalyst, and the micro-tree uniformity of charcoal of growth is good, and purity is high, best in quality, has a good application prospect in medical science, biology and field of molecular electronics.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph adopting the micro-tree of charcoal in example 1 of the present invention.Wherein (a) is the micro-tree of charcoal of institute's deposited graphite paper marginal position, the micro-tree of charcoal that (b) is graphite paper center, and (c) is that cylindric band is preced with the micro-tree of charcoal of cap and is not preced with the micro-tree construction of charcoal of cap, the fracture apperance that figure (d) is the micro-tree of charcoal.
Fig. 2 is the crystalline phase figure adopting the micro-tree of charcoal in example 2 of the present invention.The crystalline phase figure that Fig. 2 (a) is nodular texture for the crystalline phase figure of the micro-tree of independent charcoal, Fig. 2 (b);
Fig. 3 is the structural representation of settling chamber of the present invention.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Detailed description of the invention
Embodiment 1
Utilize propylene as carbon-source gas, utilize hydrogen as carrier gas, the volume ratio of propylene and hydrogen is 1:3, passes into from the air inlet 8 bottom vertical heater 1, is the micro-tree 3 of deposit carbon on the graphite paper of 30 μm at thickness.As substrate on the inwall that graphite paper is attached to settling chamber's graphite tube.The diameter of the micro-tree of charcoal is 150-200 μm, and length is 0.5-1.5mm(Fig. 1).Vertical cylinder graphite resistor furnace utilizes insulation quilt 3 to be incubated, and between flat-temperature zone, 6 is 100mm × 300mm, and the heating-up temperature of heater 3 is 850 ° of C; absorption graphite rod 4 diameter is 15mm; length is 180mm, and air pressure is a standard atmospheric pressure, and hydrogen is as the protective atmosphere of the cooling overall process that heats up.Final reaction product is discharged by gas outlet 2.Fig. 1 is the scanning electron microscope (SEM) photograph of the micro-tree of prepared charcoal.Graphite paper is prepared the micro-tree of charcoal and is mainly divided into two kinds of structures: the micro-tree construction of charcoal (Fig. 1 a and Fig. 1 b) of fine and close warty carbon structure and cylindric band hat cap, wherein the former is the early structure of the latter.(Fig. 1 a) and the charcoal micro-tree construction of center (Fig. 1 b) prepared by position is even, degree of orientation is better at graphite paper edge.The top of the micro-tree of charcoal has hat hat shape carbon structure, and along with the prolongation of sedimentation time, the hat cap of the micro-tree of charcoal starts to adsorb carbon black, becomes roughening greatly (Fig. 1 c).Fracture apperance shows that the center of the micro-tree of charcoal is made up of (Fig. 1 d) a series of concentric layered shell polysaccharide pyrolytic carbon being difficult to distinguish.
The pattern of the micro-tree of the charcoal deposited is shown in Fig. 1, and the structural representation of settling chamber is shown in Fig. 3.
Embodiment 2
Utilize methane as carbon-source gas, utilize hydrogen as carrier gas, the volume ratio of methane and hydrogen is 1:5, passes into from the air inlet 8 bottom vertical heater 1, in the micro-tree 5 of isostatic pressing formed graphite deposited on silicon charcoal.Isostatic pressing formed graphite is processed into graphite tube as substrate.The diameter of the micro-tree of charcoal is 50 μm, and length is 1.4mm.
Vertical cylinder graphite resistor furnace utilizes insulation quilt 7 to be incubated, and between flat-temperature zone, 6 is 100mm × 300mm, and the heating-up temperature of heater 3 is 940 ° of C; the diameter of absorption graphite rod 4 is 20mm; length is 210mm, pressure-fired, and hydrogen is as the protective atmosphere of the cooling overall process that heats up.Final reaction product is discharged by gas outlet 2.Fig. 2 is that (Fig. 2 a) and the crystalline phase figure of warty carbon structure (Fig. 2 b) for the prepared micro-tree of charcoal.As seen from the figure, the micro-tree of charcoal has significantly hat cap feature (Fig. 2 a), take growth cone as foundation (Fig. 2 b), is made up of the charcoal shell of the thin-line-shaped carbon structure in center and outside Turbostratic.
Embodiment 3
Utilize natural gas as carbon-source gas, utilize hydrogen as carrier gas, the volume ratio of natural gas and hydrogen is 1:8, passes into from the air inlet 8 bottom vertical heater 1, has the micro-tree 5 of charcoal of certain size at graphite paper deposited on silicon.As substrate on the inwall that graphite paper is attached to settling chamber's graphite tube.Vertical cylinder graphite resistor furnace utilizes insulation quilt 7 to be incubated, and between flat-temperature zone, 6 is 100mm × 300mm, and the heating-up temperature of heater 3 is 1000 ° of C, absorption graphite rod
4diameter be 25mm, length is 240mm, pressure-fired, hydrogen as heat up cooling overall process protective atmosphere.Final reaction product is by gas outlet
2discharge.
Claims (4)
1. the preparation method of the micro-tree of charcoal, it is characterized in that: by carbon-source gas, utilize hydrogen as carrier gas, pass into bottom vertical heater in settling chamber, the micro-tree of deposition growing charcoal in 850-1000 ° of C constant temperature space, the ratio of carbon-source gas and hydrogen is 1:(3 ~ 8), settling chamber is the graphite piece of tubular, and substrate is placed on the inwall of graphite tube; Settling chamber's central mounting has a device adsorbing carbon black, and the device of described absorption carbon black is graphite rod, and the diameter of graphite rod is the 15-25% of diameter between effective flat-temperature zone, and length is the 60-80% of height between effective flat-temperature zone.
2. the preparation method of the micro-tree of charcoal according to claim 1, it is characterized in that: described substrate is smooth pyrolytic carbon, pyrolytic graphite, graphite paper or isostatic pressing formed graphite substrate, wherein pyrolytic carbon and pyrolytic graphite are deposited on graphite tube inwall as substrate, graphite paper is attached to graphite tube inwall as substrate, and isostatic pressing formed graphite is directly processed into graphite tube as substrate.
3. the preparation method of the micro-tree of charcoal according to claim 1, is characterized in that: carbon-source gas is methane, natural gas or propylene.
4. the preparation method of the micro-tree of charcoal according to claim 3, is characterized in that: the volume ratio of propylene and hydrogen is 1:(4 ~ 6).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410666985.1A CN104451960B (en) | 2014-11-20 | 2014-11-20 | A kind of preparation method of the micro-tree of charcoal |
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| CN201410666985.1A CN104451960B (en) | 2014-11-20 | 2014-11-20 | A kind of preparation method of the micro-tree of charcoal |
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| CN104451960A true CN104451960A (en) | 2015-03-25 |
| CN104451960B CN104451960B (en) | 2016-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591797A (en) * | 2016-11-23 | 2017-04-26 | 东莞劲胜精密组件股份有限公司 | Method for quickly coating carbon film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676664A (en) * | 2004-04-01 | 2005-10-05 | 中南大学 | Method for rapidly preparing carbon/carbon composite material under physics field by CVD |
| WO2011060621A1 (en) * | 2009-11-20 | 2011-05-26 | 中南大学 | Process and device for improving properties of carbon paper with chemical vapor infiltration coating quickly applied by pressure-gradient method |
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2014
- 2014-11-20 CN CN201410666985.1A patent/CN104451960B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676664A (en) * | 2004-04-01 | 2005-10-05 | 中南大学 | Method for rapidly preparing carbon/carbon composite material under physics field by CVD |
| WO2011060621A1 (en) * | 2009-11-20 | 2011-05-26 | 中南大学 | Process and device for improving properties of carbon paper with chemical vapor infiltration coating quickly applied by pressure-gradient method |
Non-Patent Citations (2)
| Title |
|---|
| W.G. ZHANG ET AL.: "《Chemical vapor infiltration of carbon fiber felt: optimization of densification and carbon microstructure》", 《CARBON》, vol. 40, 31 December 2002 (2002-12-31), pages 2529 - 2545 * |
| 谢志勇等: "《CVI炭/炭复合材料微观结构和生长模型》", 《中国有色金属学报》, vol. 17, no. 7, 31 July 2007 (2007-07-31), pages 1096 - 1100 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591797A (en) * | 2016-11-23 | 2017-04-26 | 东莞劲胜精密组件股份有限公司 | Method for quickly coating carbon film |
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| CN104451960B (en) | 2016-08-24 |
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