CN104555988B - A kind of chemical vapour deposition technique produces method and the application of micron order diameter carbon line - Google Patents
A kind of chemical vapour deposition technique produces method and the application of micron order diameter carbon line Download PDFInfo
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- CN104555988B CN104555988B CN201510040668.3A CN201510040668A CN104555988B CN 104555988 B CN104555988 B CN 104555988B CN 201510040668 A CN201510040668 A CN 201510040668A CN 104555988 B CN104555988 B CN 104555988B
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Abstract
The present invention relates to a kind of method producing the micron-sized carbon line of diameter of chemically based vapour deposition, belong to chemical vapour deposition technique field. Powdered graphite doped with Si powder Yu SiO 2 powder is put in porcelain boat, the porcelain boat being placed with Si powder, SiO 2 powder and powdered graphite is heated in the environment of full argon hydrogen gaseous mixture, after heating, the environment of full argon hydrogen gaseous mixture is cooled to room temperature and porcelain boat is taken out. The invention provides the new way of large-scale production micron order diameter carbon line application, have the advantages that cost is low, raw material simple, be suitable for industrial mass production. Compared with the existing CNT synthesized, having length long, diameter is thick, the feature that mechanics rigidity is strong. To build at micro element, microelectrode makes, have more application in microcircuit protection.
Description
Technical field
The present invention relates to a kind of chemical vapour deposition technique and produce method and the application of micron order diameter carbon line, belong to micro-nano structure synthesis and application.
Background technology
Micron and the structure of nano-scale dimension, can show many physical propertys being different from macroscopic material. Synthesize more novel micron and nanometer sized materials, it is possible to produce the microstructure based on different elements and device for exploring. Usual carbon line is defined as: generate based on carbon, has nanometer or micron order radial dimension, and axial dimension is in or more than micron-sized a kind of structure. These structures often have good mechanical characteristic and electrology characteristic, are people's focal points of developing nano material of future generation. Chemical vapour deposition technique refers to when reacting substance A is subject to necessarily heating for a long time, and chemical reaction can be occurred to obtain product B, is deposited on the solid substrate surface of heating. Generally we use the reacting substance of solid-state, after having solid-state to become gaseous state, series of chemical occur and cools down subsequently, again becoming solid after being heated under certain condition. When different, add different reacting substances, it is possible to generate different products. Along with constantly groping reaction condition and reacting substance, diversified microstructure can be generated with chemical vapour deposition technique.
After CNT and Graphene etc. are suggested based on the microstructure of carbon, owing to they have the performance of excellence on mechanics with electrical properties, many researchs focus on the application prospect of the aspects such as the electricity of these peacekeeping two-dimensional structures and mechanics. Simultaneously in order to synthesize a greater variety of microstructure based on carbon, relevant synthetic method experienced by unremitting exploration and trial. Having been able to synthesize the CNT of various different nanometer scale diameter at present, the synthetic method related to has arc discharge method, laser ablation method, chemical vapour deposition technique, catalystic pyrolysis etc. These little to several nanometer of linear material radial dimensions, greatly to hundreds of nanometer. Pipe range and diameter proportion, more than 1000:1, are the desirable fibrous materials of material engineering teacher, have good toughness with elastic.But this smaller carbon line structure has bigger difficulty in actual applications. And keeping pipe range and diameter ratio under the premise more than 1000:1, pursue that size is bigger, there is well collimated with mechanical toughness, be easier to the carbon line handled, and realize the processing to micro element by this carbon line, become the further goal to fight for of needs.
The development through certain time of micro-manipulation field and microelectrode field, has occurred in that the mature technology utilizing gold, silver metallics composition microprobe. But, this kind of probe is it is generally required to Precision Machining obtains, relatively costly, and diameter is difficult to by industrialized operation processing to less than 10 microns. Inhibition is brought to the extensive development of correlation technique and popularization. And CNT receives the concern of people because of its outstanding mechanical property. Make and a kind of less costly, Stability Analysis of Structures, dependable performance, size are prone to processing and the carbon line structure used, it is possible to efficiently solve this problem. Current microelectrode is widely used in biological cell field, compared to metal electrode, utilizes the electrode that carbon line makes can largely avoid cyto-architectural damage. Therefore there is good market application foreground.
Summary of the invention
The invention aims to solve the problem that the carbon line of existing Nano grade size is difficult to apply to micro-manipulation, it is proposed to a kind of chemical vapour deposition technique produces method and the application of micron order diameter carbon line.
It is an object of the invention to be achieved through the following technical solutions.
A kind of chemical vapour deposition technique produces the method for micron order diameter carbon line, and step is as follows:
Step one, Si powder, SiO 2 powder and powdered graphite are 1:1:10 mix homogeneously according to mol ratio after, be fully ground, put on clean, dry ceramic vessel. The central authorities that ceramic vessel is placed in tube furnace quartz ampoule;
Step 2, passing into carrier gas, carrier gas is the gaseous mixture of argon and hydrogen, and carrier gas flux is 3～9SCCM; It is warming up to 1300 DEG C, heating 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 average 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 vapour deposition technique produces the application of micron order diameter carbon line
The carbon line obtained is applied in micro Process, concrete application process: carbon line one end is connected with metal probe and fixes, then metal probe is fixed on micro-bench board. Mobile micro-bench board, utilizes the operation that the nano wire on silicon chip or object stage, nano belt structure are moved, rotate by carbon line;
The carbon line obtained is applied to microelectrode field, concrete application process: carbon line is connected with metal electrode and fixes with elargol, and metal electrode is placed on microoperation platform. Then microoperation platform is utilized to go to control carbon line close to the region needing measurement, after touching, fixing probe location, it is operated by platform and applies to measure voltage, do the measurement of voltage-current curve.
Beneficial effect
1, a kind of chemical vapour deposition technique of the present invention produces micron order diameter carbon line compared with existing one-dimensional CNT, it is easier to realize microscopic manipulation, making suitable in microprobe, microelectrode, it is possible to realize many application in biological cell field and micro element field.
2, the method that a kind of chemical vapour deposition technique of the present invention produces micron order diameter carbon line, synthetic method has the advantages that cost is low, raw material sources extensive, be prone to industrialized production.
3, the method that a kind of chemical vapour deposition technique of the present invention produces micron order diameter carbon line, the carbon line synthesized has good collimation, electric conductivity, and the length of easily manipulation and mechanical toughness. Can be widely applied to micro structure processing, the field such as microelectrode making.
Accompanying drawing explanation
Fig. 1 is the bright field image obtained in embodiment 1;
Fig. 2 is the image observed with colorful CCD camera in embodiment 1;
Fig. 3 is the Raman image measured in embodiment 1;
Fig. 4 is the SEM image obtained in embodiment 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the summary of the invention of the present invention is further described.
Embodiment 1
A kind of chemical vapour deposition technique 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 with transmission electron microscope (TEM) or scanning electron microscope (SEM) institute within 10% with energy disperse spectroscopy.
A kind of chemical vapour deposition technique produces the method for micron order diameter carbon line
It is 1:1:10 uniform stirring 10 minutes in mortar by silica fume powder, SiO 2 powder and powdered graphite according to mol ratio; Ceramic vessel dehydrated alcohol cleans 10 minutes in ultrasonic washing instrument, dry in drying baker, cleans quartz ampoule standby. Then the mixture of powder, SiO 2 powder and powdered graphite is put into ceramic vessel, until powder upper surface and ceramic vessel upper surface being maintained an equal level, then by powder upper surface compacting. And ceramic vessel is placed on the central authorities of quartz ampoule. Quartz ampoule is put into tube furnace, the upstream elder generation connection traffic meter of quartz ampoule, connecting gas extraction system, downstream connects exhaust treatment system, pass into the gaseous mixture of argon and hydrogen again, after aerofluxus one hour, throughput is adjusted to 6sccm, begin to warm up, being heated to 1300 DEG C after 15 minutes, constant temperature, after one hour, closes tube furnace, continue ventilation, until being cooled to room temperature, having carbon line to generate at powder surface, the carbon line average diameter obtained is 1.5 μm, axial length is about 1.5cm on average, along airflow direction Parallel Growth; There is on ceramic vessel surface one layer of atrament to generate, obtain silvery reflection flaky substance at the tube wall place at 11 centimetres of airflow downstream places of distance center warm area simultaneously. Ceramic vessel is taken out from tube furnace, with tweezers, scattered carbon line is put on the silicon chip of cleaning, is put into basis of microscopic observation shape appearance figure as shown in fig. 1. The carbon line average diameter obtained is 1.5 μm, and axial length is about 1.5cm on average, as shown in Figure 2. The Raman spectrum of carbon line is as it is shown on figure 3, the characteristic peak of two graphite occurred at 1360 and 1580 places proves that it belongs to graphite-structure. SEM image proves that it has very good collimation, as shown in Figure 4.
A kind of chemical vapour deposition technique produces the application of micron order diameter carbon line
The carbon line obtained is applied in micro-manipulation, concrete application process: carbon line one end is connected with metal probe and fixes, then metal probe is fixed on micro-bench board. Being placed on clean silicon chip by monodispersed cadmium sulfide nano wires sample, silicon chip is put under the microscope. Mobile micro-bench board, utilizes the bottom of the mid portion of nano wire on carbon line contact silicon chip, and traveling probe makes cadmium sulfide nano wires be pressed on carbon line. The operations such as the position of metal probe and carbon line, and then cadmium sulfide nano wires is moved by realization, rotation are controlled according to required requirement.
The carbon line obtained is applied to microelectrode field, concrete application process: carbon line is connected with metal electrode and fixes with elargol, and metal electrode is fixed on microoperation platform.Being placed on clean silicon chip by monodispersed silver wire sample, silicon chip is put under the microscope. Then utilize microoperation platform to remove the carbon line controlling to be separately fixed on positive and negative metal electrode so that it is close to silver wire two ends or other want measure region, after touching, with controller, metal probe is applied required voltage, does the measurement of voltage-current curve.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not the restriction to embodiments of the present invention. Every belong to apparent change that technical scheme extended out or the variation row still in protection scope of the present invention.
Claims (1)
1. the method that a chemical vapour deposition technique produces micron order diameter carbon line, it is characterised in that: specifically comprise the following steps that
Step one, Si powder, SiO 2 powder and powdered graphite are 1:1:10 mix homogeneously according to mol ratio after, be fully ground, put on clean, dry ceramic vessel; The central authorities that ceramic vessel is placed in tube furnace quartz ampoule;
Step 2, passing into carrier gas, carrier gas is the gaseous mixture of argon and hydrogen, and carrier gas flux is 3～9sccm; It is warming up to 1300 DEG C, heating 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 average 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.
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