CN105692592A - Method for preparing orientated-growth carbon nanofiber array - Google Patents
Method for preparing orientated-growth carbon nanofiber array Download PDFInfo
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- CN105692592A CN105692592A CN201610252987.5A CN201610252987A CN105692592A CN 105692592 A CN105692592 A CN 105692592A CN 201610252987 A CN201610252987 A CN 201610252987A CN 105692592 A CN105692592 A CN 105692592A
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- fiber array
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- tagger
- growth carbon
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002134 carbon nanofiber Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 239000010949 copper Substances 0.000 claims abstract description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 19
- 239000004917 carbon fiber Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 13
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000006073 displacement reaction Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 6
- 238000004381 surface treatment Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000003708 ampul Substances 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 6
- 229910052573 porcelain Inorganic materials 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract 5
- 229910052751 metal Inorganic materials 0.000 abstract 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 239000010408 film Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 7
- 239000000835 fiber Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910021392 nanocarbon Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention provides a method for preparing an orientated-growth carbon nanofiber array. First, a displacing method is utilized for generating a layer of copper film on the surface of a thin metal plate in a displacing mode, namely, the thin metal plate is subjected to surface treatment, a copper sulfate water solution is prepared as displacement liquid, the thin metal plate is soaked into the copper sulfate water solution for 5-8 seconds at normal temperature, and then a layer of copper film is generated on the surface of the thin metal plate; then with the copper film formed on the metal substrate being a catalyst and acetylene gas being carbon source atmosphere, heating is performed inside quartz tubes of a heating furnace, reaction is kept for constant-temperature time of 18-22 minutes, then heating is stopped, and after natural cooling, the orientated-growth carbon fiber array can be obtained. The method is easy to implement, reaction conditions are mild and controllable, raw materials are easy to obtain, the method is safe and reliable, the size of the catalyst is even and stable, catalyzing efficiency is high, and the obtained carbon fiber array is arranged regularly and combined with the substrate well, is uniform in diameter and large in length-diameter ratio and achieves orientated growth.
Description
Technical field
The present invention relates to technical field of nano material, the preparation method particularly relating to a kind of oriented growth carbon nano-fiber array。
Background technology
After CNT in 1991 is found, people begin with destination and prepare carbon nano-fiber。The diameter of carbon nano-fiber, between CNT and gas-phase growth of carbon fibre, not only has the character of gas-phase growth of carbon fibre, and similar with CNT in properity and application etc.。
Carbon nano-fiber majority is to be prepared by catalysis pyrolysis hydrocarbon gas, it is easy to realize industrialized production。Carbon nano-fiber not only has the character that general material with carbon element has, and also has the advantage such as low-density, corrosion-resistant, high temperature resistant aging resistance, and meanwhile, carbon nano-fiber also has mechanical property and the electrical property of uniqueness, for instance high ratio modulus, high specific strength, high conductivity。Premium properties due to carbon nano-fiber, it is expected to as catalyst base, lithium rechargeable battery anode material, electrical double layer capacitor electrodes, high-efficiency adsorbent, separating medium, structural reinforcement material, stealth material, electromagnetic shielding material or darkroom absorbing material etc., and in hydrogen storage, nm-class conducting wire etc., has potential use。
Catalyst is extremely important in the preparation of carbon nano-fiber and carbon pipe, in all factors affecting carbon fiber and the growth of carbon pipe, catalyst size is one of key factor, and many research work are devoted to develop the effective catalyst being conducive to large-scale production Nano carbon fibers peacekeeping carbon pipe。Reaction temperature is most important equally for the controllable growth of carbon nanomaterial。
Chemical gaseous phase evaporation prepares carbon nano-fiber array technique, has the advantage of its uniqueness, is easier to realize。No matter how intensive array carbon nanotube, the growth that they are always vertical in substrate, here it is the self-steering growth often mentioned or self-assembled growth。It has been generally acknowledged that this growth of carbon nano-fiber is due to Van der Waals reciprocal action, the only possible direction of growth that so intensive carbon nano-fiber causes can only be vertically up。Therefore, realize this dense arrangement growth it is crucial that prepare intensive active catalyst particle at substrate surface。
How can effectively control the aligned growth state of carbon fiber array, then be the present invention problem of needing solution badly。
Summary of the invention
It is an object of the invention to utilize the suprabasil uniform copper film of ferrum to make catalyst, it is provided that the preparation method of the oriented growth carbon nano-fiber array of a kind of simple possible, provide new way for oriented growth carbon fiber array。
For solving above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The preparation method of a kind of oriented growth carbon nano-fiber array, specifically adopts following steps:
(1) catalyst is first prepared, by standby after tagger surface treatment, then copper sulfate solution is configured, using this solution as displacement liquid, tagger after process immerses in described copper sulfate solution, carries out displacement reaction, and reaction temperature is room temperature, dip time is 5-8 second, obtains the surface tagger with nanometer copper mold；
(2) take the surface that a certain amount of step 1) prepares and be placed in porcelain boat with the tagger of copper mold, porcelain boat is put into the quartz ampoule of heating furnace, to quartz ampoule evacuation, be subsequently passed carbon-source gas acetylene to atmospheric pressure；
(3) begin to warm up, after heating occurs to reaction, keep constant temperature time 18-22 minute, then turn off heating；
(4) take out product after naturally cooling to room temperature, obtain carbon nano-fiber array。
Further, in step (1), described tagger acetone and dilute hydrochloric acid carry out surface treatment。
Further, the concentration of described copper sulfate solution is 0.2-0.25mol/L。
Further, in step (1), displacement reaction temperature is 20-30 DEG C。
Further, in step (4), the type of cooling is furnace cooling。
Further, in described copper film, the particle diameter of nanoparticle is 200-300nm。
Further, the diameter of described carbon fiber is suitable with catalyst nanoparticles particle diameter, is 200-300nm。
The carbon fiber array of the present invention is at the suprabasil copper film catalysis oriented growth of ferrum。
The present invention selects at the bottom of iron-based uniform copper thin film as catalyst, it is prepared for the carbon nano-fiber array of oriented growth, have studied the relation between the diameter of carbon fiber and nanocatalyst particles particle diameter, namely the diameter of carbon fiber is suitable with catalyst nanoparticles particle diameter, and the controlled synthesis for nano-carbon material has laid certain basis。
The carbon fiber array preparation method of the present invention, displacement reaction is utilized to generate uniform copper film at iron-based basal surface, and as catalyst, in acetylene carbon source atmosphere in quartz ampoule, it is heated to uniform temperature catalytic decomposition carbon-source gas, at substrate surface, oriented growth is carbon nano-fiber array, with linear type fiber for Main Morphology。
The carbon fiber array preparation method of the present invention, used catalyst is plating nanocrystalline Cu film。This plating nanocrystalline Cu film is with tagger for substrate, one layer of nano thin-film of displacement, even particle distribution in finite concentration copper-bath, and size uniformity is 200-300nm, and this particle size determines the diameter of single fiber in institute's grown carbon fiber array。With this thin film for catalyst, acetylene gas is carbon-source gas, and when nanofiber is prepared in chemical vapour deposition (CVD), its catalytic action is single nanometer copper particle, and this particle size does not raise with temperature and changes。The carbon nano-fiber array of growth and substrate are tightly combined, it is simple to preserve and collect。
The carbon fiber array preparation method of the present invention, prepared array density is big, and between single fiber, arrangement is closely, no significant defect, and length is consistent, uniform particle sizes。
The carbon fiber array preparation method of the present invention, whole process grows in carbon source atmosphere, and raw material is pure, free from admixture。
Compared with prior art, advantages of the present invention and having the benefit effect that
The preparation method of the present invention is simple to operate, and reaction condition gentleness is controlled, and raw material easily obtains, safe and reliable, catalyst size is uniform and stable, and catalytic efficiency is high, and obtained carbon fiber array arrangement is regular, is well combined with substrate, diameter is homogeneous, and draw ratio is big, oriented growth。
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the SEM photograph of iron-based bed load copper film；
Fig. 2 is the SEM photograph of prepared carbon nano-fiber array；
Fig. 3 is the TEM photo of prepared carbon nano-fiber array；
Fig. 4 is the XRD photo of prepared carbon nano-fiber array。
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further detailed explanation。Should be appreciated that embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention。
The embodiment of the present invention is the preparation method of a kind of oriented growth carbon nano-fiber array, one layer of copper film is generated at tagger surface replacement first with displacement method, namely tagger is carried out surface treatment, compound concentration is that the copper sulfate solution of 0.2mol/L is as displacement liquid, under room temperature (20-30 DEG C), the time of tagger immersion copper sulfate solution is 5-8 second, and at one layer of copper film of Surface Creation of tagger, in copper film, the particle diameter of nanoparticle is 200-300nm；Then with load at the suprabasil copper film of ferrum for catalyst, with acetylene gas for carbon source atmosphere, heat in the quartz ampoule of heating furnace, keep reaction constant temperature time 18-22 minute, then turn off heating, natural cooling can obtain the carbon fiber array of oriented growth。
Being prepared by of the catalyst of the present invention is standby after first tagger surface acetone and dilute hydrochloric acid being processed, then copper sulfate solution is configured, using this solution as displacement liquid, tagger after process immerses in copper sulfate solution, carries out displacement reaction, and reaction temperature is room temperature (20-30 DEG C), time is 5-8 second, the preparation method of this catalyst is very simple, and catalyst size is uniform and stable, and catalytic efficiency is high。
The following examples are describing in further detail the present invention。
First, tagger is cut into the sample of 1 × 2cm, processes surface with acetone and dilute hydrochloric acid respectively。
Then, configuration concentration is the copper sulfate solution of 0.2mol/L, and during by the iron plate after process at room temperature 20-30 DEG C, impregnation process was taken out after 6 seconds, naturally dried。Fig. 1 is the SEM photograph of iron-based bed load copper film, and the preparation method of this catalyst is simple to operate, and reaction condition gentleness is controlled, and raw material easily obtains, safe and reliable, and catalyst size is uniform and stable。
Then, the substrate handled well is placed in the porcelain boat of 80 × 20mm, puts in the quartz ampoule of heating furnace, to quartz ampoule evacuation, then passing into acetylene gas, heating furnace is warmed up to the temperature starting reaction, keep constant temperature time 20min, then turn off heating, with stove natural cooling。
Fig. 2, Fig. 3 are SEM and the TEM photo of prepared carbon nano-fiber array；Fig. 4 is the XRD photo of prepared carbon nano-fiber array。
The diameter of carbon fiber prepared by the present embodiment is suitable with catalyst nanoparticles particle diameter, and for 200-300nm, length is micron order, and major part keeps directed simple interest form preferably。
From the photo of Fig. 2,3,4, adopt the carbon nano-fiber array density that the preparation method of the present invention prepares big, arrange between single fiber regular closely, be well combined with substrate, no significant defect, diameter is homogeneous, and length is consistent, draw ratio is big, oriented growth, uniform particle sizes。
The above, be only presently preferred embodiments of the present invention, is not the restriction that the present invention makees other form, and any those skilled in the art are changed or be modified as the Equivalent embodiments of equivalent variations possibly also with the technology contents of the disclosure above。But every without departing from technical solution of the present invention content, according to any simple modification, equivalent variations and remodeling that above example is made by the technical spirit of the present invention, still fall within the protection domain of technical solution of the present invention。
Claims (7)
1. the preparation method of an oriented growth carbon nano-fiber array, it is characterised in that adopt following steps:
(1) catalyst is first prepared, by standby after tagger surface treatment, then copper sulfate solution is configured, using this solution as displacement liquid, tagger after process immerses in described copper sulfate solution, carries out displacement reaction, and reaction temperature is room temperature, dip time is 5-8 second, obtains the surface tagger with nanometer copper mold；
(2) take the surface that a certain amount of step 1) prepares and be placed in porcelain boat with the tagger of copper mold, porcelain boat is put into the quartz ampoule of heating furnace, to quartz ampoule evacuation, be subsequently passed carbon-source gas acetylene to atmospheric pressure；
(3) begin to warm up, after heating occurs to reaction, keep constant temperature time 18-22 minute, then turn off heating；
(4) take out product after naturally cooling to room temperature, obtain carbon nano-fiber array。
2. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: in step (1), described tagger acetone and dilute hydrochloric acid carry out surface treatment。
3. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: the concentration of described copper sulfate solution is 0.2-0.25mol/L。
4. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: in step (1), displacement reaction temperature is 20-30 DEG C。
5. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: in step (4), the type of cooling is furnace cooling。
6. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: in described copper film, the particle diameter of nanoparticle is 200-300nm。
7. the preparation method of oriented growth carbon nano-fiber array according to claim 1, it is characterised in that: the diameter of described carbon fiber is 200-300nm。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081324A (en) * | 2018-07-27 | 2018-12-25 | 青岛科技大学 | A kind of preparation method of racemosus shape carbon fiber/amorphous carbon composite material |
| CN115385327A (en) * | 2022-08-30 | 2022-11-25 | 青岛科技大学 | In-situ preparation method and continuous growth device of carbon material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950925A (en) * | 2014-05-13 | 2014-07-30 | 青岛科技大学 | Preparation method of nano graphite flakes |
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2016
- 2016-04-22 CN CN201610252987.5A patent/CN105692592A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950925A (en) * | 2014-05-13 | 2014-07-30 | 青岛科技大学 | Preparation method of nano graphite flakes |
Non-Patent Citations (1)
| Title |
|---|
| 于立岩: "一维碳纳米材料的可控制备及其生长机理的研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081324A (en) * | 2018-07-27 | 2018-12-25 | 青岛科技大学 | A kind of preparation method of racemosus shape carbon fiber/amorphous carbon composite material |
| CN109081324B (en) * | 2018-07-27 | 2021-09-17 | 青岛科技大学 | Preparation method of multi-dendritic carbon fiber/amorphous carbon composite material |
| CN115385327A (en) * | 2022-08-30 | 2022-11-25 | 青岛科技大学 | In-situ preparation method and continuous growth device of carbon material |
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Application publication date: 20160622 |