CN104555988A - Method for producing micron-diameter carbon wires by using chemical vapor deposition method and application - Google Patents
Method for producing micron-diameter carbon wires by using chemical vapor deposition method and application Download PDFInfo
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- CN104555988A CN104555988A CN201510040668.3A CN201510040668A CN104555988A CN 104555988 A CN104555988 A CN 104555988A CN 201510040668 A CN201510040668 A CN 201510040668A CN 104555988 A CN104555988 A CN 104555988A
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Abstract
The invention relates to a method for producing micron-diameter carbon wires by using a chemical vapor deposition method, which belongs to the filed of chemical vapor deposition technologies. The method comprises the following steps: putting silicon powder and silicon dioxide powder doped graphite powder in a porcelain boat, heating the porcelain boat in which silicon powder, silicon dioxide powder and graphite powder are put in an environment filled with argon-hydrogen mixed gas, then cooling the porcelain boat to room temperature in the environment filled with argon-hydrogen mixed gas, and taking out the porcelain boat. The invention provides a new way for the large-scale production and application of micron-diameter carbon wires. The method has the characteristics of low cost, simple materials, and is suitable for industrial mass production. Compared with the existing synthesized carbon nanotubes, the micron-diameter carbon wires has the characteristics of long length, large diameter, and strong mechanical rigidity, and therefore, the micron-diameter carbon wires have more applications in the aspects of micro-device construction, microelectrode manufacturing, micro-circuit protection.
Description
Technical field
The present invention relates to method and application that a kind of chemical Vapor deposition process produces micron order diameter carbon line, belong to micro-nano structure Synthesis and application field.
Background technology
Micron and the structure of nano-scale dimension, can show many physical propertiess being different from macroscopic material.Synthesize more novel micron and nanometer sized materials, may be used for exploring and produce based on the microtexture of different element and device.Usual carbon line is defined as: generate based on carbon, have nanometer or micron order radial dimension, axial dimension is in or is greater than micron-sized a kind of structure.These structures often have good mechanical characteristic and electrology characteristic, are the focal points that people develop nano material of future generation.When chemical Vapor deposition process refers to that reactive material A is subject to necessarily heating for a long time, chemical reaction can be there is and obtain product B, be deposited on the solid substrate surface of heating.Usually we use solid-state reactive material, have after heating under certain condition solid-state become gaseous state after, there is series of chemical cooling subsequently, again become solid.Under different conditions, add different reactive material, different products can be generated.Along with constantly groping reaction conditions and reactive material, diversified microtexture can be generated with chemical Vapor deposition process.
After carbon nanotube and Graphene etc. are suggested based on the microtexture of carbon, because they have excellent performance on mechanics and electrical properties, much research focuses on the application prospect of the aspects such as the electricity of these peacekeeping two-dirnentional structures and mechanics.Simultaneously in order to synthesize a greater variety of microtexture based on carbon, relevant synthetic method experienced by unremitting exploration and trial.Can synthesize the carbon nanotube of various different nanometer scale diameter at present, the synthetic method related to has arc discharge method, laser ablation method, chemical Vapor deposition process, catalystic pyrolysis etc.These linear material radial dimensions are little of a few nanometer, greatly to hundreds of nanometer.Pipe range and diameter proportion, more than 1000:1, are the filamentary materials that material engineering teacher is desirable, have good toughness and elasticity.But the carbon line structure that this size is less has larger difficulty in actual applications.And keeping pipe range and diameter ratio more than under the prerequisite of 1000:1, pursue size larger, have well collimated and mechanical toughness, be easier to the carbon line handled, and realize the processing to micro element by this carbon line, become and need further goal to fight for.
Micro-manipulation field and microelectrode field, through the development of certain hour, have occurred utilizing gold and silver metallics to form the mature technology of microprobe.But this kind of probe generally needs precision sizing to obtain, and cost is higher, and diameter is difficult to be machined to less than 10 microns by industrialized operation.Inhibition is brought to the extensive development of correlation technique and popularization.And carbon nanotube receives the concern of people because of its outstanding mechanical property.Make that a kind of cost is lower, Stability Analysis of Structures, dependable performance, size are easy to process and the carbon line structure used, can effectively address this problem.Current microelectrode is widely used in biomass cells field, and compared to metal electrode, the electrode utilizing carbon line to make can be avoided to a great extent to cyto-architectural damage.Therefore there is good market application foreground.
Summary of the invention
The carbon line that the object of the invention is to solve existing Nano grade size is difficult to the problem being applied to micro-manipulation, proposes method and application that a kind of chemical Vapor deposition process produces micron order diameter carbon line.
The object of the invention is to be achieved through the following technical solutions.
Chemical Vapor deposition process produces a method for micron order diameter carbon line, and step is as follows:
Step one, be, after 1:1:10 mixes, fully grind Si powder, SiO 2 powder and powdered graphite according to mol ratio, put on clean, dry earthenware porcelain receptacle.Earthenware porcelain receptacle is placed in the central authorities of tube furnace silica tube;
Step 2, pass into carrier gas, carrier gas is the gas mixture of argon gas and hydrogen, and carrier gas flux is 3 ~ 9SCCM; Be warming up to 1300 DEG C, temperature rise rate is 60 ~ 70 DEG C/min, insulation 3 ~ 5h, close tube furnace, continue logical carrier gas, be cooled to room temperature, long straight micron order diameter carbon line is obtained on mixed powder surface, the carbon line trunk mean diameter obtained is 1 μm ~ 5 μm, axial length average out to 1cm-2cm, and all carbon lines are all along air current flow direction Parallel Growth.
A kind of chemical Vapor deposition process produces the application of micron order diameter carbon line
The carbon line obtained is applied in micro Process, embody rule method: carbon line one end is connected with metal probe and fixes, then metal probe is fixed on micro-operation desk.Mobile micro-operation desk, utilizes the operation that carbon line moves the nano wire on silicon chip or Stage microscope, nano belt structure, rotates;
The carbon line obtained is applied to microelectrode field, embody rule method: carbon line be connected with metal electrode and fix with elargol, and being placed on micro-operation platform by metal electrode.Then utilize micro-operation platform to go to control carbon line close to the region needing to measure, after touching, stationary probe position, applies measuring voltage by operator's console, does the measurement of voltage-current curve.
Beneficial effect
1, a kind of chemical Vapor deposition process of the present invention produces micron order diameter carbon line compared with existing one dimension carbon nanotube, more easily realize microscopic manipulation, be applicable to the making of microprobe, microelectrode, many application in biomass cells field and micro element field can be realized.
2, a kind of chemical Vapor deposition process of the present invention produces the method for micron order diameter carbon line, synthetic method has that cost is low, raw material sources extensively, be easy to the feature of suitability for industrialized production.
3, a kind of chemical Vapor deposition process of the present invention produces the method for micron order diameter carbon line, and the carbon line synthesized has good collimation, electroconductibility, and the length of easily manipulation and mechanical toughness.Microstructure processing can be widely used in, the fields such as microelectrode making.
Accompanying drawing explanation
Fig. 1 is the bright field image obtained in embodiment 1;
Fig. 2 is with the image that colorful CCD camera is observed in embodiment 1;
Fig. 3 is the Raman image measured in embodiment 1;
Fig. 4 is the SEM image obtained in embodiment 1.
Embodiment
Below in conjunction with drawings and Examples, summary of the invention of the present invention is further described.
Embodiment 1
A kind of chemical Vapor deposition process produces micron order diameter carbon line, this carbon line is the graphite-structure doped with silicon (Si), calculate with total amount of substance of this material, the molar content of silicon can be characterized within 10% with transmission electron microscope (TEM) or scanning electron microscope (SEM) institute band energy spectrometer.
A kind of chemical Vapor deposition process produces the method for micron order diameter carbon line
Be 1:1:10 uniform stirring 10 minutes in mortar by silica fume powder, SiO 2 powder and powdered graphite according to mol ratio; Earthenware porcelain receptacle dehydrated alcohol cleans 10 minutes in ultrasonic washing instrument, and dry in loft drier, cleaning silica tube is for subsequent use.Then the mixture of powder, SiO 2 powder and powdered graphite is put into earthenware porcelain receptacle, until powder upper surface and earthenware porcelain receptacle upper surface are maintained an equal level, then by the compacting of powder upper surface.And earthenware porcelain receptacle is placed on the central authorities of silica tube.Silica tube is put into tube furnace, the first connection traffic meter in upstream of silica tube, in connection exhaust system, downstream connects flare system, pass into the gas mixture of argon gas and hydrogen again, be vented after one hour, airshed is adjusted to 6sccm, start heating, be heated to 1300 DEG C after 15 minutes, constant temperature, after one hour, closes tube furnace, continue ventilation, until cool to room temperature, have carbon line to generate at powder surface, the carbon line mean diameter obtained is 1.5 μm, axial length is about 1.5cm on average, along air flow line Parallel Growth; There is one deck atrament to generate on earthenware porcelain receptacle surface, obtain silvery reflection flaky substance at the tube wall place at distance center warm area 11 centimetres of airflow downstream places simultaneously.Earthenware porcelain receptacle is taken out from tube furnace, with tweezers, the carbon line of dispersion is put on clean silicon chip, is put into basis of microscopic observation shape appearance figure as shown in fig. 1.The carbon line mean diameter obtained is 1.5 μm, and axial length is about 1.5cm on average, as shown in Figure 2.As shown in Figure 3, the characteristic peak of two graphite occurred at 1360 and 1580 places proves that it belongs to graphite-structure to the Raman spectrum of carbon line.SEM image proves that it has very good collimation, as shown in Figure 4.
A kind of chemical Vapor deposition process produces the application of micron order diameter carbon line
The carbon line obtained is applied in micro-manipulation, embody rule method: carbon line one end is connected with metal probe and fixes, then metal probe is fixed on micro-operation desk.Be placed on clean silicon chip by monodispersed cadmium sulfide nano wires sample, silicon chip is put under the microscope.Mobile micro-operation desk, utilize carbon line to contact the bottom of the middle portion of the nano wire on silicon chip, traveling probe makes cadmium sulfide nano wires be pressed on carbon line.Control the position of metal probe and carbon line according to required requirement, so realize moving cadmium sulfide nano wires, the operation such as rotation.
The carbon line obtained is applied to microelectrode field, embody rule method: carbon line be connected with metal electrode and fix with elargol, and being fixed on micro-operation platform by metal electrode.Be placed on clean silicon chip by monodispersed silver-colored line sample, silicon chip is put under the microscope.Then utilize micro-operation platform to go to control to be separately fixed at the carbon line on positive and negative metal electrode, make it want the region measured close to silver-colored line two ends or other, after touching, with controller, required voltage is applied to metal probe, do the measurement of voltage-current curve.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (2)
1. chemical Vapor deposition process produces a method for micron order diameter carbon line, it is characterized in that: concrete steps are as follows:
Step one, be, after 1:1:10 mixes, fully grind Si powder, SiO 2 powder and powdered graphite according to mol ratio, put on clean, dry earthenware porcelain receptacle; Earthenware porcelain receptacle is placed in the central authorities of tube furnace silica tube;
Step 2, pass into carrier gas, carrier gas is the gas mixture of argon gas and hydrogen, and carrier gas flux is 3 ~ 9SCCM; Be warming up to 1300 DEG C, temperature rise rate is 60 ~ 70 DEG C/min, insulation 3 ~ 5h, close tube furnace, continue logical carrier gas, be cooled to room temperature, long straight micron order diameter carbon line is obtained on mixed powder surface, the carbon line trunk mean diameter obtained is 1 μm ~ 5 μm, axial length average out to 1cm-2cm, and all carbon lines are all along air current flow direction Parallel Growth.
2. chemical Vapor deposition process produces an application for micron order diameter carbon line, it is characterized in that: the method that carbon line is applied in micro Process is: be connected with metal probe carbon line one end and fix, then is fixed on by metal probe on micro-operation desk; Mobile micro-operation desk, utilizes the operation that carbon line moves the nano wire on silicon chip or Stage microscope, nano belt structure, rotates;
The method that carbon line is applied in microelectrode field is: carbon line be connected with metal electrode and fix with elargol, and being placed in by metal electrode on micro-operation platform; Then utilize micro-operation platform to go to control carbon line close to the region needing to measure, after touching, stationary probe position, applies measuring voltage by operator's console, does the measurement of voltage-current curve.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842142A (en) * | 2018-07-03 | 2018-11-20 | 河北工业大学 | A kind of film and preparation method thereof being made of micron order pentagon stannous oxide |
| CN112510180A (en) * | 2020-12-02 | 2021-03-16 | 江苏科技大学 | Silicon oxide-carbon filament active material and preparation method and application thereof |
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| US6541113B1 (en) * | 1998-07-24 | 2003-04-01 | Cabot Corporation | Methods for preparing silica-coated carbon products |
| CN1915805A (en) * | 2005-08-19 | 2007-02-21 | 清华大学 | Device and method for preparing array of Nano carbon tube |
| WO2009104202A1 (en) * | 2008-02-19 | 2009-08-27 | Indian Institute Of Technology | Device and method to use single walled carbon nanotube composites for gas sensing applications |
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Patent Citations (3)
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|---|---|---|---|---|
| US6541113B1 (en) * | 1998-07-24 | 2003-04-01 | Cabot Corporation | Methods for preparing silica-coated carbon products |
| CN1915805A (en) * | 2005-08-19 | 2007-02-21 | 清华大学 | Device and method for preparing array of Nano carbon tube |
| WO2009104202A1 (en) * | 2008-02-19 | 2009-08-27 | Indian Institute Of Technology | Device and method to use single walled carbon nanotube composites for gas sensing applications |
Non-Patent Citations (2)
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| 杨晓安等: "碳纤维纳米微电极制作技术与噪声分析", 《现代电子技术》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842142A (en) * | 2018-07-03 | 2018-11-20 | 河北工业大学 | A kind of film and preparation method thereof being made of micron order pentagon stannous oxide |
| CN112510180A (en) * | 2020-12-02 | 2021-03-16 | 江苏科技大学 | Silicon oxide-carbon filament active material and preparation method and application thereof |
| CN112510180B (en) * | 2020-12-02 | 2021-11-09 | 江苏科技大学 | Silicon oxide-carbon filament active material and preparation method and application thereof |
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