CN102557004B - Method for controlling growth appearance of carbon nanometer material through magnetic field - Google Patents
Method for controlling growth appearance of carbon nanometer material through magnetic field Download PDFInfo
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- CN102557004B CN102557004B CN201110440769.1A CN201110440769A CN102557004B CN 102557004 B CN102557004 B CN 102557004B CN 201110440769 A CN201110440769 A CN 201110440769A CN 102557004 B CN102557004 B CN 102557004B
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Abstract
The invention relates to a method for controlling growth appearance of a carbon nanometer material through a magnetic field, which comprises the following steps: taking a magnetic metal material sputtered on a silicon chip as a catalyst, heating a hollow graphite tube by using a high-frequency induction coil, at the same time, providing an alternating magnetic field, putting the silicon chip on which the catalyst is sputtered into the hollow graphite tube and heating for 5-30 minutes to obtain the carbon nanometer material of which the appearance is controlled by the magnetic filed. The zigzag carbon nanometer material is prepared by the alternating magnetic field. Compared with the prior art, carbon nanometer materials with different appearances can be obtained through changing the size and the direction of the magnetic field.
Description
Technical field
The invention belongs to carbon nanomaterial preparation field, especially relate to a kind of method by Magnetic control growth appearance of carbon nanometer material.
Background technology
Since Japanese Scientists Iijima in 1991 finds carbon nanotube, large quantities of scientific worker has carried out large quantifier elimination to one-dimensional carbon nano material.Carbon nanomaterial mainly comprises the carbon nanotube of diameter below 100 nanometers and the carbon nanofiber of diameter below 500 nanometers, and its length can reach tens of or hundreds of micron.Due to the structural performance of its uniqueness, make it have unusual physics, chemistry and mechanical property etc., be considered in one dimension transmitter, the field such as superpower matrix material, superhard material, hydrogen storage material, catalyzer and support of the catalyst, high-efficiency adsorbent, absorbing material has broad application prospects, and is subject to the attention of Many researchers.But the growth morphology controlling carbon nanomaterial by external environment seldom has report, especially utilizes magnetic field never to appear in the newspapers to the growth morphology controlling carbon nanomaterial.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and provide a kind of magnetic field that utilizes to control the method for growth appearance of carbon nanometer material, in the process of growth of carbon nanomaterial, changed the growth morphology of carbon nanomaterial by the size and Orientation changing magnetic field.
Object of the present invention can be achieved through the following technical solutions:
By a method for Magnetic control growth appearance of carbon nanometer material, comprise the following steps:
(1) on silicon chip, sputter one deck magnetic metal material or magnetic metal oxide material;
(2) silicon chip through above-mentioned process is placed in hollow graphite pipe, this hollow graphite pipe is located in silica tube, and is placed in radio-frequency coil sphere of action;
(3) hollow graphite pipe is vacuumized, then pass into hydrogen and organic carbon gas, open the power supply of radio-frequency coil, after reaction for some time, silicon chip obtains black product, is the carbon nanomaterial of specific morphology.
Magnetic metal material described in step (1) is iron, cobalt, nickel or for its alloy.
Magnetic metal oxide material described in step (1) is the oxide compound of iron, cobalt or nickel.
Magnetic metal material described in step (1) or magnetic metal oxide sputtering of materials thickness are 10-300nm.
Described radio-frequency coil makes carbon tube be rapidly heated and provides alternating magnetic field.
Organic carbon gas described in step (3) is methane or acetylene, and the hydrogen flowing quantity passed into is 10-50sccm, and the organic carbon gas flow passed into is 30-200sccm.
The volume ratio that hydrogen and organic carbon gas pass into preferably 1: 3.
Reaction times used in step (3) is 5-30 minute.
It is 750-900 DEG C that step (3) medium-high frequency coil controls temperature of reaction, and internal magnetic field is alternating magnetic field, and produced by the exchange current in coil, frequency is 30KHz-60KHz.
Key of the present invention is, the radio-frequency induction coil used not only can produce the high-frequency vortex coaxial with hollow graphite pipe, thus carbon tube is rapidly heated, also the high-frequency alternating magnetic field of carbon tube axis can be produced, above-mentioned inducedmagnetic field can control the trend of magnetic catalyst, thus reaches the growth morphology controlling carbon nanomaterial.
The growth mechanism of carbon nanomaterial prepared by the present invention: one of them the important growth mechanism preparing one-dimensional material is VLS mechanism (gas-solid-liquid mechanism), the key of this mechanism is the droplet-like catalyzer being positioned at one-dimensional material top or bottom, catalyzer is at high temperature melted into droplet-like, drop constantly adsorbs the gas in atmosphere in Material growth process, when the material in drop reaches supersaturation, material is separated out becomes solid, drop continued dissolution gas and precipitation, thus grow up to one-dimensional material.The present invention adopts iron, cobalt, and the magneticsubstances such as nickel, as catalyzer, guarantee to follow VLS growth mechanism growth of one-dimensional carbon nanomaterial on the one hand, magnetic field also can be utilized to carry out the trend of inducing catalyst on the one hand, thus control the pattern of carbon nanomaterial.
Compared with prior art, the present invention is by the size and Orientation of controlling magnetic field, the carbon nanomaterial of various different-shape can be obtained, adopt iron, cobalt, the magneticsubstances such as nickel, as catalyzer, guarantee to follow VLS growth mechanism growth of one-dimensional carbon nanomaterial on the one hand, also magnetic field can be utilized to carry out the trend of inducing catalyst on the other hand, thus control the pattern of carbon nanomaterial.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the class zigzag carbon nanomaterial that the present invention prepares.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
1, on the silicon chip cleaned, sputter one deck iron, sputtering time is 10-50 second, and thickness is approximately 30-300 nanometer;
2, above-mentioned silicon chip is placed in hollow graphite pipe, and is placed in the sphere of action of radio-frequency induction coil, whole carbon tube is placed in airtight silica tube; Open vacuum pump, start to vacuumize, make vacuum tightness in silica tube reach about 10Pa, pass into hydrogen, hydrogen flowing quantity is 30sccm;
3, bleeding regulating amount, make can keep pressure in silica tube, open radio-frequency induction coil power supply, carbon tube temperature reached about 750 degree within 1 minute, reach temperature required after, continue to pass into hydrogen 2 minutes, make institute's sputter material on silicon chip be reduced into metal simple-substance, then pass into acetylene, flow is 90sccm.
5, keep temperature, keep the flow of hydrogen and acetylene, react 15 minutes, powered-down;
6, after naturally cooling, silicon chip can obtain a large amount of atrament, the carbon nanomaterial grown under being Magnetic control.
In the present embodiment, magnetic field used is produced by ruhmkorff coil, and magnetic field is the alternating magnetic field along carbon tube axis, and the carbon nanomaterial therefore obtained is class zigzag, as shown in Figure 1.
Embodiment 2
Splash-proofing sputtering metal changes nickel and cobalt into, and the organic carbon gas passed into changes methane into, temperature requiredly changes 900 degree into, and all the other are constant, can obtain the flexuose carbon nanomaterial of class equally.
Embodiment 3
By a method for Magnetic control growth appearance of carbon nanometer material, comprise the following steps:
(1) on silicon chip, sputter one deck ferric oxide as catalyzer, metal oxide materials sputtering thickness is 10nm;
(2) silicon chip through above-mentioned process is placed in hollow graphite pipe, this hollow graphite pipe is located in silica tube, and is placed in radio-frequency coil sphere of action, and radio-frequency coil makes carbon tube be rapidly heated and provides alternating magnetic field;
(3) hollow graphite pipe is vacuumized, then hydrogen and methane is passed into, hydrogen flowing quantity is 10sccm, and the flow of methane is 30sccm, then opens the power supply of radio-frequency coil, controlling temperature of reaction is 750 DEG C, the frequency controlling radio-frequency coil is 30KHz, for inside provides high-frequency alternating magnetic field, and reaction 30min, silicon chip obtains black product, is the carbon nanomaterial of specific morphology.
Embodiment 4
By a method for Magnetic control growth appearance of carbon nanometer material, comprise the following steps:
(1) on silicon chip, sputter one deck cobalt oxide as catalyzer, metal oxide materials sputtering thickness is 50nm;
(2) silicon chip through above-mentioned process is placed in hollow graphite pipe, this hollow graphite pipe is located in silica tube, and is placed in radio-frequency coil sphere of action, and radio-frequency coil makes carbon tube be rapidly heated and provides alternating magnetic field;
(3) hollow graphite pipe is vacuumized, then hydrogen and methane is passed into, hydrogen flowing quantity is 30sccm, and the flow of methane is 100sccm, then opens the power supply of radio-frequency coil, controlling temperature of reaction is 800 DEG C, the frequency controlling radio-frequency coil is 50KHz, for inside provides high-frequency alternating magnetic field, and reaction 15min, silicon chip obtains black product, is the carbon nanomaterial of specific morphology.
Embodiment 5
By a method for Magnetic control growth appearance of carbon nanometer material, comprise the following steps:
(1) on silicon chip, sputter one deck ferrocobalt as catalyzer, metal oxide materials sputtering thickness is 50nm;
(2) silicon chip through above-mentioned process is placed in hollow graphite pipe, this hollow graphite pipe is located in silica tube, and is placed in radio-frequency coil sphere of action, and radio-frequency coil makes carbon tube be rapidly heated and provides alternating magnetic field;
(3) hollow graphite pipe is vacuumized, then hydrogen and acetylene is passed into, hydrogen flowing quantity is 50sccm, and the flow of acetylene is 200sccm, then opens the power supply of radio-frequency coil, controlling temperature of reaction is 900 DEG C, the frequency controlling radio-frequency coil is 60KHz, for inside provides high-frequency alternating magnetic field, and reaction 5min, silicon chip obtains black product, is the carbon nanomaterial of specific morphology.
Claims (8)
1., by a method for Magnetic control growth appearance of carbon nanometer material, it is characterized in that, the method comprises the following steps:
(1) on silicon chip, sputter one deck magnetic metal material or magnetic metal oxide material;
(2) silicon chip through above-mentioned process is placed in hollow graphite pipe, this hollow graphite pipe is located in silica tube, and is placed in radio-frequency coil sphere of action;
(3) hollow graphite pipe is vacuumized, then pass into hydrogen and organic carbon gas, open the power supply of radio-frequency coil, after reaction for some time, silicon chip obtains black product, is the carbon nanomaterial of specific morphology;
It is 750-900 DEG C that step (3) medium-high frequency coil controls temperature of reaction, and radio-frequency coil provides inner alternating magnetic field, and the frequency that radio-frequency coil controls is 30KHz-60KHz.
2. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, is characterized in that, the magnetic metal material described in step (1) is iron, cobalt, nickel or be its alloy.
3. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, it is characterized in that, the magnetic metal oxide material described in step (1) is the oxide compound of iron, cobalt or nickel.
4. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, it is characterized in that, the magnetic metal material described in step (1) or magnetic metal oxide sputtering of materials thickness are 10-300nm.
5. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, it is characterized in that, described radio-frequency coil makes carbon tube be rapidly heated and provides alternating magnetic field.
6. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, it is characterized in that, organic carbon gas described in step (3) is methane or acetylene, and the hydrogen flowing quantity passed into is 10-50sccm, and the organic carbon gas flow passed into is 30-200sccm.
7. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1 or 6, is characterized in that, the preferred 1:3 of volume ratio that hydrogen and organic carbon gas pass into.
8. a kind of method by Magnetic control growth appearance of carbon nanometer material according to claim 1, it is characterized in that, the reaction times used in step (3) is 5-30 minute.
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| CN108646793B (en) * | 2018-04-04 | 2020-12-25 | 山西大学 | Device and method for controlling three-dimensional shape of two-dimensional material |
| CN113078038B (en) * | 2021-03-23 | 2022-06-07 | 电子科技大学 | Large-current cold cathode of oriented carbon nanotube and preparation method thereof |
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