CN101722000B - Preparation method of high-efficiency composite catalyst film for overlength carbon nano tube growth - Google Patents
Preparation method of high-efficiency composite catalyst film for overlength carbon nano tube growth Download PDFInfo
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- CN101722000B CN101722000B CN2008102347552A CN200810234755A CN101722000B CN 101722000 B CN101722000 B CN 101722000B CN 2008102347552 A CN2008102347552 A CN 2008102347552A CN 200810234755 A CN200810234755 A CN 200810234755A CN 101722000 B CN101722000 B CN 101722000B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 10
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 229910017135 Fe—O Inorganic materials 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 238000005477 sputtering target Methods 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 43
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 13
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract 1
- 238000001755 magnetron sputter deposition Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 40
- 238000005516 engineering process Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000005289 physical deposition Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000002079 double walled nanotube Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention provides a preparation method of a high-efficiency composite catalyst film for overlength carbon nano tube growth; a silicon base is cleaned firstly and is dried by blowing, and then the silicon base is placed in a reaction chamber of a reaction magnetron sputtering device, before being deposited, the absolute pressure of the back bottom of the reaction chamber is lower than 5*10-3Pa; Fe and Mg targets are used as sputtering targets, or Fe and Al targets are adopted as sputtering targets, Ar and O2 are used as sputtering gas, and the flow ratio of the Ar and O2 is controlled between 1 and 10, after the temperature of the silicon base is heated to 200-700 DEG C, the sputtering gas is led in from the reaction chamber to a settling chamber, after the whole pressure intensity reaches 1-10Pa, sputtering film formation is carried out, the sputtering power is controlled between 40 and 100W, the vertical distance of the target and the substrate is 50-100mm, the deposited film thickness is controlled to be from 1 to 5nm; after the deposition is carried out, the temperature is cooled to be room temperature along with the furnace, a gas source is cut off, a finished product is taken out, so as to obtain Mg-Fe-O or Al-Fe-O catalyst film; the method can prepare the high-efficiency catalyst film in a large-area way, the efficiency is high, the cost is low, therefore, the preparation method is suitable for batch preparation of a carbon nano tube array.
Description
Technical field
The present invention relates to a kind of preparation and be used for the overlength carbon nano pipe method of the efficient composite catalyst film of growth fast, belong to the carbon nanotube preparation technology field.
Background technology
CNT (CNTs) has received people's extensive concern owing to having excellent physics and chemical property since 1991 come to light.The preparation method of CNTs has arc discharge, laser ablation method, chemical vapour deposition technique (CVD) etc., and chemical vapour deposition technique (CVD) is with low cost, be easy to the large tracts of land film forming, therefore is widely used.Adopt the CVD method can obtain different types of CNTs material, from the powder to the film, from individual tubes to the pipe array, from horizontally to vertical-growth etc.One of key technology of CNTs material C VD preparation is the controlled preparation of nanocatalyst, and wherein, the composition of catalyst, size and activity will play conclusive effect to structure and the pattern of growth in situ CNTs.
In order to obtain orthotropic CNTs array, some catalyst films such as one deck Fe, Co or Ni of need on backing material, growing in advance adopt physical deposition method or chemical deposition to prepare.But, heating up with stove at film catalyst and to change in the process of catalyst granules or group bunch, activity of such catalysts can reduce, and causes lower CNTs growth rate and short CNTs array.Recently, Hata group has reported the method for a kind of quick growth CNTs, is employed on the silicon substrate+Al
2O
3The method of transition zone+Fe catalyst film has prepared the long CNTs array of 2.5mm.Research thinks that the adding of cushion can stop the counterdiffusion of Fe and Si, and in heat treatment process subsequently, forms the bigger surface topography of roughness, thereby helps the even dispersion of catalyst granules or group bunch.
In sum, research preparation composite catalyst film is used for the growth of CNTs material, has the important techniques meaning.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of overlength carbon nano pipe preparation method of the efficient composite catalyst film of growth fast that is used for is provided.
The object of the invention is realized through following technical scheme:
Be used for the preparation method of the efficient composite catalyst film of overlength carbon nano tube growth, characteristics are: after earlier silicon substrate being cleaned, and dry up, put into the reative cell of reaction magnetocontrol sputtering device, reative cell back of the body end absolute pressure is lower than 5 * 10 before the deposition
-3Pa; Adopt metal Fe and Mg target as sputtering target, or adopt metal Fe and Al target as sputtering target, with Ar gas and O
2Gas is as sputter gas, Ar gas and O
2The flow-ratio control of gas is between 1～10; After treating that the silicon substrate temperature is heated to 200～700 ℃, sputter gas is introduced reative cell to the settling chamber, after overall pressure reaches 1～10Pa; The beginning spatter film forming; Sputtering power is controlled between 40～100W, and the vertical interval of target and substrate is 50～100mm, and the control thickness of deposited film is at 1～5nm; Deposition cools to room temperature with the furnace after accomplishing, and cuts off gas source, takes out finished product, thereby obtains Mg-Fe-O or Al-Fe-O catalyst film.
Further, the preparation method of the above-mentioned efficient composite catalyst film that is used for overlength carbon nano tube growth, silicon substrate is earlier with acetone, clean, use at last the deionized water ultrasonic waves for cleaning with ethanol again, cleans then to dry up with nitrogen gun.
Further, the preparation method of the above-mentioned efficient composite catalyst film that is used for overlength carbon nano tube growth, the purity of said metal Fe, Al and Mg target is higher than 99.99%.
Again further, the preparation method of the above-mentioned efficient composite catalyst film that is used for overlength carbon nano tube growth, the purity of said Ar gas is higher than 99.999%, said O
2The purity of gas is higher than 99.99%.
Substantive distinguishing features and obvious improvement that technical scheme of the present invention is outstanding are mainly reflected in:
The present invention adopts reaction magnetocontrol sputtering physical deposition legal system to be equipped with composite catalyst film; Through the processing of substrate surface, technological parameter (like atmosphere component and flow-rate ratio, growth temperature, sputtering power etc.) the acquisition efficient composite catalyst film of control in the thin film growth process.Direct growth Mg-Fe-O or Al-Fe-O composite catalyst film need not to add cushion on the silicon substrate, and the simple and catalyst of technology has active preferably.The even distribution of the favourable catalyst component of this film stops its gathering under hot conditions, thereby helps the quick growth of CNT.Utilize this catalyst to carry out the growth of CNT, can obtain average caliber and be 7～15 nanometers, length and can be 100um～1cm, double-walled or multi-walled carbon nano-tubes that tube wall is smooth.One-step method, large-area preparation efficient catalytic agent film, efficient is higher, and preparation cost is lower, is applicable to the prepared in batches of carbon nano pipe array, and market prospects are wide.
Description of drawings
Below in conjunction with accompanying drawing technical scheme of the present invention is described further:
Fig. 1: the CNT array scanning Electronic Speculum collection of illustrative plates that adopts the Mg-Fe-O composite catalyst film to obtain.
The specific embodiment
The present invention adopts reaction magnetocontrol sputtering physical deposition legal system to be equipped with Mg-Fe-O or Al-Fe-O composite catalyst film.Silicon substrate earlier with acetone, clean, use the deionized water ultrasonic waves for cleaning at last with ethanol again, is dried up with nitrogen gun after the cleaning again, put into the reative cell of reaction magnetocontrol sputtering device immediately, reative cell is carried on the back end absolute pressure and is lower than 5 * 10 before guaranteeing to deposit
-3Pa.Adopt elemental metals Fe, Al and Mg target that purity is superior to 99.99wt% as sputtering target, purity is superior to 99.999% Ar gas and purity and is superior to 99.99% O
2As sputtering atmosphere.When preparation Mg-Fe-O catalyst film, pack into Fe and Mg metal targets; And when preparation Al-Fe-O catalyst film, then pack into Fe and Al metal targets.Ar gas and O
2Gas imports reative cell, Ar gas and O by conduit after fully mixing
2(like Ar gas is 24sccm, O between 4～8 in the flow-ratio control of gas
2Be 4sccm); After treating that underlayer temperature is heated to 200～700 ℃ temperature range, sputter gas is introduced reative cell to the settling chamber, after overall pressure reaches 1～10Pa; The beginning spatter film forming; Sputtering power is controlled between 40～100W, and the vertical interval of target and substrate is 50～100mm, and thickness of deposited film is controlled between 1～5nm.After deposition process is accomplished, after sample cools to room temperature with the furnace, cut off gas source, take out sample, thereby obtain Mg-Fe-O or Al-Fe-O catalyst film.
Through the processing of substrate surface, technological parameter (like atmosphere component and flow-rate ratio, growth temperature, sputtering power etc.) the acquisition efficient composite catalyst film of control in the thin film growth process.Direct growth Mg-Fe-O or Al-Fe-O composite catalyst film need not to add cushion on the silicon substrate, and the simple and catalyst of technology has active preferably.One-step method, large-area preparation efficient catalytic agent film, efficient is higher.
Embodiment 1:
After silicon substrate (face is oriented to (111) or (100) outward) employing acetone, ethanol and deionized water ultrasonic waves for cleaning, dry up with nitrogen gun again, put into the reative cell of reaction magnetocontrol sputtering device immediately, reative cell back of the body end absolute pressure is lower than 5 * 10 before guaranteeing to deposit
-3Pa.Adopt metal Fe and Mg target that purity is superior to 99.99wt% as sputtering target, high-purity Ar gas and purity are superior to 99.99% O
2As sputtering atmosphere.Ar gas and O
2Gas imports reative cell, Ar gas and O by conduit after fully mixing
2(Ar gas is 10-100sccm, O 4 in the flow-ratio control of gas
2Be 5-50sccm), treat that underlayer temperature is heated to 200 ℃ after, sputter gas is introduced reative cell to the settling chamber; After overall pressure reaches 10Pa, the beginning spatter film forming, sputtering power is controlled between 40-100W; The vertical interval of target and substrate is 100mm, and thickness of deposited film is controlled at 1-5nm.After deposition process is accomplished, after sample cools to room temperature with the furnace, cut off gas source, take out sample, thereby obtain the Mg-Fe-O catalyst film.The CNT array scanning Electronic Speculum collection of illustrative plates of Mg-Fe-O composite catalyst film, as shown in Figure 1.
Embodiment 2:
After silicon substrate (face is oriented to (111) or (100) outward) employing acetone, ethanol and deionized water ultrasonic waves for cleaning, dry up with nitrogen gun again, put into the reative cell of reaction magnetocontrol sputtering device immediately, reative cell back of the body end absolute pressure is lower than 5 * 10 before guaranteeing to deposit
-3Pa.Adopt metal Fe and Al target that purity is superior to 99.99wt% as sputtering target, high-purity Ar gas and purity are superior to 99.99% O
2As sputtering atmosphere.Ar gas and O
2Gas imports reative cell, Ar gas and O by conduit after fully mixing
2(Ar gas is 10-50sccm, O 8 in the flow-ratio control of gas
2Be 2-20sccm), treat that underlayer temperature is heated to 700 ℃ after, sputter gas is introduced reative cell to the settling chamber; After overall pressure reaches 10Pa, the beginning spatter film forming, sputtering power is controlled between 40-100W; The vertical interval of target and substrate is 50mm, and thickness of deposited film is controlled at 1-5nm.After deposition process is accomplished, after sample cools to room temperature with the furnace, cut off gas source, take out sample, thereby obtain the Al-Fe-O catalyst film.
Prepare composite catalyst film through PVD based on physical gas phase deposition technology, the even distribution of the favourable catalyst component of this film stops its gathering under hot conditions, thereby helps the quick growth and the growth (more than the millimeter level) of CNT.Utilize this catalyst to carry out the growth of CNT, can obtain average caliber and be 7～15 nanometers, length and can be 100um～1cm, double-walled or multi-walled carbon nano-tubes that tube wall is smooth.This catalyst activity is high, preparation cost is low, is applicable to the prepared in batches of carbon nano pipe array.
Below only be concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.
Claims (1)
1. the preparation method who is used for the efficient composite catalyst film of overlength carbon nano tube growth; It is characterized in that: silicon substrate earlier with acetone, again with the ethanol cleaning, use the deionized water ultrasonic waves for cleaning at last; Cleaning the back dries up with nitrogen gun; Put into the reative cell of reaction magnetocontrol sputtering device, reative cell back of the body end absolute pressure is lower than 5 * 10 before the deposition
-3Pa; Adopt metal Fe and Mg target as sputtering target, or adopt metal Fe and Al target as sputtering target, the purity of said metal Fe, Al and Mg target is higher than 99.99%, with Ar gas and O
2Gas is as sputter gas, and the purity of said Ar gas is higher than 99.999%, said O
2The purity of gas is higher than 99.99%, Ar gas and O
2The flow-ratio control of gas is between 1～10; After treating that the silicon substrate temperature is heated to 200～700 ℃, sputter gas is introduced reative cell to the settling chamber, after overall pressure reaches 1～10Pa; The beginning spatter film forming; Sputtering power is controlled between 40～100W, and the vertical interval of target and substrate is 50～100mm, and the control thickness of deposited film is at 1～5nm; Deposition cools to room temperature with the furnace after accomplishing, and cuts off gas source, takes out finished product, thereby obtains Mg-Fe-O or Al-Fe-O catalyst film.
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| CN101722000B true CN101722000B (en) | 2012-01-11 |
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| CN112791225A (en) * | 2019-11-14 | 2021-05-14 | 美国发现集团有限公司 | Nano robot for tumor treatment and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354042A (en) * | 2001-10-31 | 2002-06-19 | 清华大学 | Titanium dioxide photocatalysis air-cleaning film and its preparation method |
| CN1460543A (en) * | 2003-06-04 | 2003-12-10 | 陕西师范大学 | TiO2 nano photocatalytic stainless steel and titanium fibre thread-line and its preparation method |
| CN101069840A (en) * | 2007-06-21 | 2007-11-14 | 复旦大学 | Method for preparing visible radiation active carbon-doped nano titanium deoxid film |
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- 2008-10-29 CN CN2008102347552A patent/CN101722000B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354042A (en) * | 2001-10-31 | 2002-06-19 | 清华大学 | Titanium dioxide photocatalysis air-cleaning film and its preparation method |
| CN1460543A (en) * | 2003-06-04 | 2003-12-10 | 陕西师范大学 | TiO2 nano photocatalytic stainless steel and titanium fibre thread-line and its preparation method |
| CN101069840A (en) * | 2007-06-21 | 2007-11-14 | 复旦大学 | Method for preparing visible radiation active carbon-doped nano titanium deoxid film |
Non-Patent Citations (1)
| Title |
|---|
| 张彭义等.固定化二氧化钛膜的制备及其光催化性能.《中国环境科学》.2000,第20卷(第5期),第436-440页. * |
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