CN104451960B - A kind of preparation method of the micro-tree of charcoal - Google Patents
A kind of preparation method of the micro-tree of charcoal Download PDFInfo
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- CN104451960B CN104451960B CN201410666985.1A CN201410666985A CN104451960B CN 104451960 B CN104451960 B CN 104451960B CN 201410666985 A CN201410666985 A CN 201410666985A CN 104451960 B CN104451960 B CN 104451960B
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Abstract
The invention discloses a kind of method utilizing chemical gaseous phase deposition to prepare the micro-tree of charcoal, by carbon-source gas, utilize hydrogen as carrier gas, it is passed through bottom vertical heater in settling chamber, the micro-tree of deposition growing charcoal in 850 1000 ° of C constant temperature spaces, the ratio of carbon-source gas and hydrogen is 1:(3～8), settling chamber is the graphite piece of tubular, and matrix is placed on the inwall of graphite tube；Settling chamber's central mounting has the device of an absorption carbon black, the device of described absorption carbon black is graphite rod, the 15 25% of a diameter of effective constant temperature interval diameter of graphite rod, the 60 80% of a length of effective constant temperature interval height, prepare a diameter of 50 200 microns, the micro-tree of charcoal of a length of 0.5 1.5 millimeters.The present invention is not introduced into catalyst, and charcoal micro-tree purity of growth is high, and quality better has a good application prospect in medical science, biology and field of molecular electronics.
Description
Art
The present invention relates to the preparation method of a kind of chemical gaseous phase deposition micro-tree of 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,
It is widely used in biomedical and field of molecular electronics.But the micro-tree of charcoal prepared by conventional method typically requires introducing metal and urges
Agent, the catalyst in the micro-tree of charcoal often cannot thoroughly be removed.Biomedical and molectronics generally requires high-quality charcoal
Micro-tree, most important of which standard is exactly purity and the uniformity of the micro-tree of charcoal.Introduce and produce the charcoal that the preparation good purity of uniformity is high
Micro-tree material becomes the technical bottleneck of association area.
Summary of the invention
Under conditions of it is an object of the invention to utilize chemical gaseous phase to be deposited on and do not introduce catalyst, growth is prepared uniform
The micro-tree of charcoal, effectively achieves the micro-tree construction of charcoal and the optimization of performance.
The present invention is realized by the following method goal of the invention:
A kind of preparation method for the purpose of the preparation high-purity micro-tree of uniform charcoal, utilizes carbon-source gas and carrier gas (hydrogen),
Grow the micro-tree of charcoal at 850-1000 ° of C which deposit on different substrates, be 1:(3～8 by controlling the ratio of carbon-source gas and hydrogen).
Substrate is positioned on the inwall of graphite tube (settling chamber).In the position being positioned at central authorities of settling chamber, being provided with carbon black adsorbent equipment, carbon black is inhaled
The 15-25% of a diameter of effective constant temperature interval diameter of adsorption device, the 60-80% of a length of effective constant temperature interval height.
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, and graphite paper can be attached to graphite tube inwall as substrate, isostatic pressed
Graphite can directly be processed into graphite tube as substrate.
The present invention is not introduced into catalyst, and charcoal micro-tree uniformity of growth is good, and purity is high, best in quality, at medical science, biology
Have a good application prospect with field of molecular electronics.
Accompanying drawing explanation
Fig. 1 is to use the scanning electron microscope (SEM) photograph of the micro-tree of charcoal in present example 1.Wherein (a) is institute's deposited graphite paper margin location
The micro-tree of charcoal put, (b) is the micro-tree of charcoal of graphite paper center, and (c) is the micro-tree of charcoal of cylindric band hat cap and is not preced with cap
The micro-tree construction of charcoal, figure (d) is the fracture apperance of the micro-tree of charcoal.
Fig. 2 is to use the crystalline phase figure of the micro-tree of charcoal in present example 2.Fig. 2 (a) is the crystalline phase figure of the micro-tree of single charcoal, Fig. 2
B () is the crystalline phase figure of nodular texture；
Fig. 3 is the structural representation of settling chamber of the present invention.
The present invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings.
Detailed description of the invention
Embodiment 1
Utilizing propylene as carbon-source gas, utilizing hydrogen is 1:3 as the volume ratio of carrier gas, propylene and hydrogen, from vertical
Air inlet 8 bottom heating furnace 1 is passed through, and deposits the micro-tree of charcoal 3 on the graphite paper that thickness is 30 μm.Graphite paper is attached to settling chamber's stone
As substrate on the inwall of ink cylinder.A diameter of 150-200 μm of the micro-tree of charcoal, a length of 0.5-1.5mm(Fig. 1).Vertical cylinder stone
Ink resistance furnace utilizes insulation quilt 3 to be incubated, and constant temperature interval 6 is 100mm × 300mm, and the heating-up temperature of heater 3 is 850 ° of C, inhales
Graphite rod 4 a diameter of 15mm, a length of 180mm, air pressure is a standard atmospheric pressure, and hydrogen is as the cooling overall process that heats up
Protective atmosphere.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 made
The standby micro-tree of charcoal is broadly divided into two kinds of structures: charcoal micro-tree construction (Fig. 1 a and the figure of cap be preced with by fine and close warty carbon structure and cylindric band
1b), wherein the former is the early structure of the latter.Charcoal micro-tree knot prepared by graphite paper edge (Fig. 1 a) and center (Fig. 1 b) position
Structure is uniform, degree of orientation is preferable.The top of the micro-tree of charcoal has hat hat shape carbon structure, along with the prolongation of sedimentation time, the hat of the micro-tree of charcoal
Cap starts to adsorb carbon black, becomes the most roughening (Fig. 1 c).Fracture apperance show the center of the micro-tree of charcoal by a series of be difficult to differentiate between same
Central layer shape pyrolytic carbon composition (Fig. 1 d).
The pattern of the micro-tree of charcoal deposited is shown in Fig. 1, and the structural representation of settling chamber is shown in Fig. 3.
Embodiment 2
Utilizing methane as carbon-source gas, utilizing hydrogen is 1:5 as the volume ratio of carrier gas, methane and hydrogen, from vertical
Air inlet 8 bottom heating furnace 1 is passed through, and deposits the micro-tree of charcoal 5 on isostatic pressing formed graphite surface.Isostatic pressing formed graphite is processed into graphite tube
As substrate.A diameter of 50 μm of the micro-tree of charcoal, a length of 1.4mm.
Vertical cylinder graphite resistor furnace utilizes insulation quilt 7 to be incubated, and constant temperature interval 6 is 100mm × 300mm, heater 3
Heating-up temperature is 940 ° of C, a diameter of 20mm of absorption graphite rod 4, a length of 210mm, pressure-fired, and hydrogen is complete as the cooling that heats up
The protective atmosphere of process.Final reaction product is discharged by gas outlet 2.The micro-tree of charcoal (Fig. 2 a) and warty charcoal that Fig. 2 is prepared are tied
The crystalline phase figure of structure (Fig. 2 b).As seen from the figure, the micro-tree of charcoal has significantly hat cap feature (Fig. 2 a), (figure with growth cone as foundation
2b), it is made up of the charcoal shell of the thin-line-shaped carbon structure in center and outside Turbostratic.
Embodiment 3
Utilizing natural gas as carbon-source gas, utilizing hydrogen is 1:8 as the volume ratio of carrier gas, natural gas and hydrogen, from
Air inlet 8 bottom vertical heater 1 is passed through, and on graphite paper surface, deposition has the micro-tree of charcoal 5 of certain size.Graphite paper pastes
As substrate on the inwall of settling chamber's graphite tube.Vertical cylinder graphite resistor furnace utilizes insulation quilt 7 to be incubated, and constant temperature interval 6 is
100mm × 300mm, the heating-up temperature of heater 3 is 1000 ° of C, a diameter of 25mm, a length of 240mm of absorption graphite rod 4, micro-
Malleation, hydrogen is as the protective atmosphere of the cooling overall process that heats up.Final reaction product is discharged by gas outlet 2.
Claims (3)
1. the preparation method of the micro-tree of charcoal, it is characterised in that: by carbon-source gas, utilize hydrogen as carrier gas, from vertical heating
Furnace bottom is passed through in settling chamber, and in 850-1000 ° of C constant temperature interval, the ratio of the micro-tree of deposition growing charcoal, carbon-source gas and hydrogen is
1:(3～8), settling chamber is the graphite piece of tubular；Settling chamber's central mounting has the device of an absorption carbon black, described adsorbent charcoal
Black device is graphite rod, the 15-25% of a diameter of effective constant temperature interval diameter of graphite rod, and a length of effective constant temperature interval is high
The 60-80% of degree；Substrate is done, wherein pyrolytic carbon and pyrolysis with smooth pyrolytic carbon, pyrolytic graphite, graphite paper or isostatic pressing formed graphite
Graphite deposits is at graphite tube inwall as substrate, or graphite paper is attached to graphite tube inwall as substrate, or isostatic pressing formed graphite is direct
It is processed into graphite tube as substrate.
The preparation method of the micro-tree of charcoal the most according to claim 1, it is characterised in that: carbon-source gas be methane, natural gas or
Propylene.
The preparation method of the micro-tree of charcoal the most according to claim 2, it is characterised 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 CN104451960A (en) | 2015-03-25 |
| CN104451960B true CN104451960B (en) | 2016-08-24 |
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| 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 (1)
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734940B (en) * | 2009-11-20 | 2012-07-25 | 中南大学 | Pressure difference-based method and device for improving properties of carbon paper of quick CVI coating |
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Patent Citations (1)
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 《Chemical vapor infiltration of carbon fiber felt: optimization of densification and carbon microstructure》;W.G. Zhang et al.;《Carbon》;20021231;第40卷;第2529-2545页 * |
| 《CVI炭/炭复合材料微观结构和生长模型》;谢志勇等;《中国有色金属学报》;20070731;第17卷(第7期);第1096-1100页 * |
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