CN112746273A - Stainless steel surface in-situ growth carbon nanofiber and preparation method thereof - Google Patents
Stainless steel surface in-situ growth carbon nanofiber and preparation method thereof Download PDFInfo
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 44
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
Abstract
The invention provides a stainless steel surface in-situ growth carbon nanofiber and a preparation method thereof. The preparation method comprises the following steps: (1) cleaning surface stains on stainless steel by using 75-100% alcohol water solution and deionized water in sequence, putting the stainless steel into a drying box, and drying at 50-100 ℃; (2) and (2) placing the stainless steel dried in the step (1) into alcohol flame for treatment, controlling the flame temperature at 700-840 ℃, and controlling the flame treatment time at 1-20min, so that the nano carbon fiber is directly deposited on the surface of the stainless steel, and the nano carbon fiber in-situ grown on the surface of the stainless steel is prepared. The preparation method has simple equipment and simple and convenient process, does not need to additionally add a catalyst, and does not need to carry out additional pretreatment steps such as polishing, acid treatment and activation on the surface of the stainless steel. The material prepared by the method can be directly used for electronic devices such as electrodes and the like.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a stainless steel surface in-situ growth nano carbon fiber and a preparation method thereof.
Background
Unlike hollow carbon nanotubes, carbon nanofibers can be viewed in their composition as solid one-dimensional nanocarbon materials made up of multiple graphene sheets arranged to have a diameter of between 10 and 500 nm. The nano carbon fiber not only has the advantages of strong conductivity, large length-diameter ratio, high specific strength, large specific modulus and the like of the traditional carbon fiber, but also has the advantages of good thermal stability, large specific surface area, few structural defects and the like. The nano carbon fiber has wide application in the fields of electrode materials, sensors, fiber composite reinforced materials, catalyst carriers, nano photoelectric materials, heavy metal ion adsorption, hydrogen storage and the like; the nano carbon fiber has the characteristics of high electron transmission speed, high active site density, strong thermal stability, high chemical stability and the like, is suitable for being applied to the fields of electronic devices, electrochemistry, conductive composite materials and the like, and has quite definite application prospect.
Common methods for preparing the carbon nanofibers comprise Chemical Vapor Deposition (CVD), solid-phase synthesis and electrostatic spinning, but have the defects of high production equipment cost, low preparation efficiency and complex preparation process; however, the flame method is a simple and economic method, can quickly and effectively produce the nano carbon material, and has the characteristics of environmental friendliness and green chemical industry.
CN1205366C discloses a method for obtaining carbon nanofibers by using carbon steel or low-carbon steel sheets containing manganese and chromium as a substrate, sequentially carrying out activation treatment such as polishing, acid leaching and the like, then carrying out treatment at 850 ℃ by a flame method, and scraping the treated carbon nanofibers, but the method needs strong acid to treat the surface of specific steel so as to increase the active points of the catalytic growth of the carbon nanofibers, and has certain problems of environmental protection and safety; and the substrate used in the method must be subjected to a previous surface polishing treatment, which makes the process difficult to use on substrates with complex shapes, such as porous structures, meshes and other woven bodies.
In addition, various catalysts such as Ni, Co, Fe salt and the like are additionally added in the preparation process of a plurality of carbon nanofibers published in the past and are coated on the surface of a substrate to serve as a source of the catalyst, the process often causes great negative effects on final products, for example, catalyst agglomeration, uneven distribution and the like which are very easy to occur in the production process often cause uneven deposition distribution of the produced carbon nanofibers, and residues of the foreign catalysts are introduced into the products; in addition, the weak bonding force between the nano carbon fibers catalytically deposited by the additional catalyst and the matrix material is also one of the problems, because the nano carbon fibers grown by the additional catalyst coated on the surface are generally difficult to ensure the strong bonding force between the nano carbon fibers and the substrate.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention mainly aims to provide a method for growing nano carbon fibers on the surface of stainless steel in situ. The method has simple equipment, does not need excessive pretreatment steps and does not need extra catalyst from the outside, and the uniformly distributed nano carbon fibers can be rapidly deposited and grown in situ on the surface of the stainless steel within dozens of minutes by utilizing the stainless steel substrate.
The second purpose of the invention is to provide the stainless steel surface in-situ growth nano carbon fiber prepared by the preparation method.
The primary purpose of the invention is realized by the following technical scheme:
a method for growing nano carbon fibers on the surface of stainless steel in situ comprises the following steps:
(1) cleaning surface stains on stainless steel by sequentially using an alcohol water solution and deionized water, putting the stainless steel into a drying box, and drying at 50-100 ℃;
(2) and (2) putting the stainless steel dried in the step (1) into alcohol flame with the volume concentration of 75-100% for treatment, controlling the flame temperature at 700-.
Further, the shape of the stainless steel is any one of a stainless steel mesh, foam, a stainless steel sheet and a stainless steel sintered felt.
Further, the step (1) is an alcohol water solution with any volume concentration.
Further, the drying temperature in the step (1) is 60 ℃.
Further, the volume concentration of the alcohol used by the flame fuel in the step (2) is 75%.
Further, the volume concentration of the alcohol used by the flame fuel in the step (2) is 100%.
Further, the temperature of the alcohol flame in the step (2) is 750 ℃.
Further, the temperature of the alcohol flame in the step (2) is 800 ℃.
Further, the burning time in the step (2) is 1-20 min.
Further, the diameter of the stainless steel surface in-situ grown carbon nanofibers prepared in the step (2) is 10-300 nm.
Further, the diameter of the stainless steel surface in-situ grown carbon nanofibers prepared in the step (2) is 10-200 nm.
The second purpose of the invention is realized by the following technical scheme:
the stainless steel surface in-situ growth carbon nanofiber prepared by the preparation method.
The mechanism of the invention is as follows:
the invention utilizes alcohol flame to carry out surface modification treatment on stainless steel, and the stainless steel is put into the alcohol flame for treatment, so that the flame treatment time is controlled to deposit and grow the nano carbon fibers with different yields on the surface of the stainless steel. Because Fe element in the stainless steel can form a catalyst for the deposition growth of the nano carbon fiber, when the stainless steel is subjected to flame treatment, the catalytic activity of the catalytic deposition nano carbon fiber can be effectively excited when the stainless steel reaches a certain treatment temperature, so that the deposition growth of the nano carbon fiber on the surface of the stainless steel is promoted. In addition, the nano carbon fiber produced by the method mainly has structures such as straight, bent and spiral structures, and the like, which are mainly caused by the fact that the crystal orientation of the catalyst iron oxide particles has anisotropy, namely the periodicity and the density degree of the metal atom arrangement along different directions of an iron oxide crystal lattice are different, so that the characteristics of catalyzing carbon deposition growth of iron oxide crystal grains in different directions are different, and the nano carbon fiber with various structures is finally produced.
The invention has the beneficial effects that:
(1) the invention utilizes the catalytic action of stainless steel, and is directly applied to the process for depositing the carbon nanofibers by flame treatment, without chemical/physical pretreatment steps such as polishing or acid washing activation and the like; the diameter of the generated carbon nanofiber is 10-300nm, the length can reach more than 2 mu m, and the carbon nanofiber can grow on foam, net-shaped, non-woven fabric or sheet-shaped stainless steel, so that the use of additional catalysts is reduced;
(2) the preparation method has the advantages of cheap used equipment, low raw material cost, simplicity and rapidness. The stainless steel substrate used in the invention is a common product in the market, the flame treatment equipment only needs alcohol flame, and the concentration of the alcohol solution can be adjusted within 75-100%.
(3) The carbon nano-products generated by the invention have various shapes. The stainless steel prepared by the invention has the advantages that the nano carbon fiber grown in situ on the surface is solid fiber instead of hollow carbon nano tube. In addition, the product of the invention has various shapes such as straight, bent, spiral and the like, which are greatly caused by the anisotropy of the catalyst and the difference of the growth modes of the catalytic carbon deposition;
(4) the invention can catalyze and deposit the carbon nanofibers through the catalytic activity of the stainless steel substrate, the bonding force between the in-situ grown carbon nanofibers and the substrate is better, the carbon nanofiber deposition efficiency is high, and the carbon nanofibers are grown and distributed on the substrate more uniformly.
Drawings
FIG. 1 is a scanning electron micrograph of an untreated 180 mesh 304 stainless steel mesh in example 1;
FIG. 2 is an SS-1min scanning electron micrograph in example 1;
FIG. 3 is an SS-20min scanning electron micrograph in example 1;
FIG. 4 is a transmission electron micrograph of the filamentous nanocarbon of example 1;
FIG. 5 is an SS-10min scanning electron micrograph in example 1;
FIG. 6 is an electrochemical CV curve of stainless steel mesh electrode with the surface deposited with nano carbon fiber under different flame treatment time in example 1;
FIG. 7 is a comparison of SS-20min in example 1 with the electrochemical specific surface area test curve of the electrode for CNFs prepared in patent (r);
FIG. 8 is a comparison of SS-20min in example 1 with the electrode capacitive energy test curve of CNFs prepared in patent (r);
FIG. 9 is an SS-75% SEM image of example 2;
FIG. 10 is a scanning electron micrograph of the surface of a 304 stainless steel sheet before and after 7min of flame treatment in example 3, wherein (a) the scanning electron micrograph of the 304 stainless steel sheet before flame treatment and (b) the scanning electron micrograph of the 304 stainless steel sheet after 7min of flame treatment.
Detailed Description
The technical solution of the present invention is further described below with reference to the specific embodiments and the accompanying drawings. The scope of the present invention is not limited to the following examples, and reagents and materials used in the present invention may be generally purchased in the market unless otherwise specified.
The following examples relate to the methods for testing and analyzing the stainless steel mesh, which mainly include yield calculation, Cyclic Voltammetry (CV), Transmission Electron Microscope (TEM), and Scanning Electron Microscope (SEM).
And (3) calculating the yield: the yield of the carbon nanofibers grown on the surface of the stainless steel by the flame method can be calculated by weighing the mass of the stainless steel before and after the treatment and by the following formula:
electrochemical testing: using electrochemical workstation instrument of Shanghai Chenghua apparatus Co., Ltd, selecting saturated calomel electrode as reference electrode, platinum sheet as counter electrode, and cutting stainless steel into 1 × 1cm2The dimensions of (a) were subjected to flame treatment and electrochemical testing. Electrolyte is 1mol/LH2SO4Or NaSO4Working electrode testingBefore the test, activation treatment is carried out, namely, result comparison is carried out after the CV curve is stabilized.
The Scanning Electron Microscope (SEM) used was a field emission scanning electron microscope of ULTRA 55, a specification of which is manufactured by ZEISS, Germany, and the Transmission Electron Microscope (TEM) used was a transmission electron microscope of JEM-2100F, a specification of which is manufactured by JEM.
Comparative example: preparing CNFs on the surface of Q235 steel according to the method of the published patent CN1205366C (patent r); with PVDF: CNFs was coated on a 180 mesh 304 stainless steel mesh used in this patent at a ratio of 1:9 as a comparative example, and the product performance was tested.
Example 1:
(1) taking 1X 1cm2Cleaning a 180-mesh 304 stainless steel net by using ethanol and deionized water, and drying in a vacuum drying oven at 60 ℃;
(2) treating the cleaned stainless steel mesh at 750 deg.C with 100% volume concentration ethanol flame, controlling flame treatment time at 1/5/10/20min, and marking the flame-treated sample as SS-1min, SS-5min, SS-10min, and SS-20 min; growing the nano carbon fiber on the surface of the stainless steel to prepare the nano carbon fiber in situ grown on the surface of the stainless steel; the yields were 0.9%, 5.0%, 6.3%, 8.3%, respectively.
The growth of the amount of active substances such as carbon and the like is rapid from 1min to 5min, and the growth trend of the nano carbon fiber tends to be gentle from 5min to 10min later.
FIG. 1 is a scanning electron microscope image of an untreated 180-mesh 304 stainless steel mesh, and FIG. 2 is a scanning electron microscope image of SS-1min, and it is evident by comparison that the carbon material uniformly distributed grows on the surface of the stainless steel mesh after the flame treatment; FIG. 3 is a scanning electron microscope image of SS-20min, compared with FIG. 2, the stainless steel surface deposits more carbon material with longer flame treatment time; the morphology of the deposited carbon nanofibers of the stainless steel surface layer can be clearly seen from fig. 4, which is a solid fiber structure with catalyst particles on the top.
FIG. 5 is an SS-5min scanning electron micrograph in which the helical filamentous nanocarbon structure can be observed.
As shown in fig. 6, the stainless steel mesh without flame treatment has low current density and poor electrochemical activity, and the electrochemical response current of the stainless steel mesh after flame treatment is greatly increased, so that the electrochemical activity is remarkably improved.
According to FIG. 7, the specific electrochemical surface area of SS-20min in example 1 is 56m2 g-1And the electrochemical specific surface area is close to that of a CNFs electrode coated by a comparative example.
The SS-20min electrode capacitance of example 1 was 58.3F g as measured from FIG. 8-1Much greater than the capacitance of the electrode made of the comparative example coated CNFs (34F g)-1)。
Example 2:
(1) taking 0.5X 0.5cm2Cleaning a 180-mesh 304 stainless steel net by using ethanol and deionized water, and drying in a vacuum drying oven at 60 ℃;
(2) treating the cleaned stainless steel mesh by using 75% ethanol flame in volume concentration at 750 ℃, and controlling the flame treatment time to be 10min, so that the nano carbon fibers grow on the surface of the stainless steel, and preparing the nano carbon fibers growing on the surface of the stainless steel in situ; the obtained product is recorded as SS-75%, and the appearance of the product is shown in figure 9.
Example 3:
(1) taking 1X 1cm2Cleaning a 304 stainless steel sheet as a substrate by ethanol and deionized water in sequence, and drying in a vacuum drying oven at 60 ℃;
(2) carrying out flame treatment on the cleaned 304 stainless steel sheet by using 100% ethanol flame in volume concentration at 750 ℃, and controlling the flame treatment time to be 7min, so that the nano carbon fibers grow on the surface of the stainless steel, and preparing the nano carbon fibers growing on the surface of the stainless steel in situ; the appearance of the flame-treated sample is shown in FIG. 10.
Example 4:
(1) taking 1X 1cm2Cleaning a 316L stainless steel sheet as a substrate by ethanol and deionized water in sequence, and drying in a vacuum drying oven at 60 ℃;
(2) and (3) treating the cleaned 316L stainless steel sheet at 800 ℃ by using 100% ethanol flame in volume concentration, and controlling the flame treatment time to be 7min, so that the nano carbon fibers grow on the surface of the stainless steel, and preparing the nano carbon fibers growing on the surface of the stainless steel in situ.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The method for growing the carbon nanofibers on the surface of the stainless steel in situ is characterized by comprising the following steps of:
(1) cleaning surface stains on stainless steel by sequentially using an alcohol water solution and deionized water, putting the stainless steel into a drying box, and drying at 50-100 ℃;
(2) and (2) putting the stainless steel dried in the step (1) into alcohol flame with the volume concentration of 75-100% for treatment, controlling the flame temperature at 700-.
2. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the stainless steel is in the shape of any one of a net, a foam, a sheet and a sintered felt.
3. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the volume concentration of alcohol in the step (2) is 75%.
4. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the volume concentration of alcohol in the step (2) is 100%.
5. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the temperature of the alcohol flame in the step (2) is 750 ℃.
6. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the temperature of the alcohol flame in the step (2) is 800 ℃.
7. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the burning time in the step (2) is 1-20 min.
8. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 1, wherein the diameter of the nano carbon fibers on the surface of stainless steel prepared in step (2) is 10-300 nm.
9. The method for growing nano carbon fibers on the surface of stainless steel in situ according to claim 8, wherein the diameter of the nano carbon fibers on the surface of stainless steel prepared in step (2) is 10-200 nm.
10. The stainless steel surface in-situ grown carbon nanofibers prepared by the preparation method of any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114093955A (en) * | 2021-10-15 | 2022-02-25 | 华南理工大学 | Gallium arsenide solar cell with carbon nanofiber doped with nickel oxide hole transport layer and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499095A (en) * | 2014-12-10 | 2015-04-08 | 哈尔滨工业大学 | Method for preparing carbon fiber yarns by direct flame carbon deposition |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499095A (en) * | 2014-12-10 | 2015-04-08 | 哈尔滨工业大学 | Method for preparing carbon fiber yarns by direct flame carbon deposition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114093955A (en) * | 2021-10-15 | 2022-02-25 | 华南理工大学 | Gallium arsenide solar cell with carbon nanofiber doped with nickel oxide hole transport layer and preparation method thereof |
| CN114093955B (en) * | 2021-10-15 | 2024-03-08 | 华南理工大学 | Gallium arsenide solar cell with carbon nanofiber doped with nickel oxide hole transport layer and preparation method of gallium arsenide solar cell |
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