CN117777506A - Preparation method and application of corrosion inhibition and wave absorption integrated film - Google Patents
Preparation method and application of corrosion inhibition and wave absorption integrated film Download PDFInfo
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- CN117777506A CN117777506A CN202410199206.5A CN202410199206A CN117777506A CN 117777506 A CN117777506 A CN 117777506A CN 202410199206 A CN202410199206 A CN 202410199206A CN 117777506 A CN117777506 A CN 117777506A
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Abstract
The invention relates to the technical field of corrosion inhibition wave-absorbing materials, and discloses a preparation method and application of a corrosion inhibition wave-absorbing integrated film. The preparation method of the corrosion inhibition and wave absorption integrated film comprises the steps of firstly preparing an RGO/CIP composite wave absorption material, then adding the RGO/CIP composite wave absorption material and a multi-element corrosion inhibitor into DMF, adding TPU after ultrasonic treatment, heating, stirring, fully dispersing uniformly, scraping and coating on a glass slide, and drying to obtain the corrosion inhibition and wave absorption integrated film. According to the invention, the graphene with dielectric loss behavior and carbonyl iron with magnetic loss behavior are effectively compounded by utilizing the coupling effect of the silane coupling agent, so that the synergistic effect of a system medium-magnetic double mechanism is realized. The existence of carbonyl iron effectively adjusts impedance mismatch of the system caused by high conductivity of graphene, and simultaneously, a large number of heterojunction surfaces formed between the carbonyl iron and the graphene introduce new interface polarization for the system, so that the electromagnetic wave absorption performance of the composite system is remarkably enhanced.
Description
Technical Field
The invention relates to the technical field of corrosion inhibition wave-absorbing materials, in particular to a preparation method and application of a corrosion inhibition wave-absorbing integrated film.
Background
The vapor phase corrosion inhibitor VCIs (Volatile Corrosion Inhibitors) can volatilize automatically at normal temperature, and is slowly adsorbed on the outer surface of metal in the form of small molecules or particles to block external harmful gas such as O 2 ，CO 2 ，SO 2 ，H 2 S and water vapor and other corrosion medium to contact the metal surface to reach the aim of rust prevention. Compared with the traditional coating, the vapor phase corrosion inhibition film can be used without complicated pretreatment steps and the like. More importantly, the vapor phase corrosion inhibitor can play a role in corrosion inhibition and protection without directly contacting with metal, so that the basic characteristics of the metal surface are maintained to the maximum extent, and the vapor phase corrosion inhibitor can be widely applied to corrosion protection of precise instruments. Meanwhile, through reasonable design of a vapor phase corrosion inhibition system, long-acting corrosion inhibition performance comparable to that of a traditional anti-corrosion coating can be realized by utilizing the synergistic effect of a plurality of corrosion inhibition mechanisms.
The high-efficiency corrosion inhibition of the VCIs can prevent the magnetic metal wave absorbing system in the composite system from corroding in a complex working environment so as to lose the wave absorbing function. Based on the method, the invention provides a plurality of components for coupling a plurality of loss mechanisms, the dielectric loss material and the magnetic loss material are compounded to realize the synergism of medium-magnetic loss, the intervention of the magnetic material can adjust the impedance matching performance of the composite material, and the heterogeneous interface constructed among the multiple components can provide new interface polarization relaxation for the material, so that the system can obtain excellent electromagnetic wave attenuation performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, solve the problems of radar detection and corrosion easiness of marine equipment and facilities, and provide a preparation method and application of a corrosion inhibition and wave absorption integrated film.
In order to achieve the aim, the technical scheme of the invention is that the preparation method of the corrosion inhibition and wave absorption integrated film comprises the following steps:
(1) Uniformly dispersing Graphene Oxide (GO) and Carbonyl Iron (CIP) in absolute ethyl alcohol;
(2) Adding dimethyl octadecyl (3-trimethoxy silicon propyl) ammonium chloride solution (DMAOP) of isopropanol to the mixed solution in the step (1), and then fully stirring the mixed solution at 800 rpm for 12 h;
(3) Carrying out suction filtration on the mixed solution after stirring in the step (2), flushing by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using sodium ascorbate (VcNa);
(5) Performing suction filtration and drying on the reduced GO/CIP composite wave-absorbing material to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding RGO/CIP composite wave-absorbing material and multi-element corrosion inhibitor into N, N-Dimethylformamide (DMF), adding Thermoplastic Polyurethane (TPU) after ultrasonic treatment, heating and stirring to fully disperse uniformly;
(7) The uniformly dispersed solution was knife coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain a corrosion inhibition and wave absorption integrated film (named RGO/CIP film).
Further; the mass ratio of GO to CIP in the step (1) is (0.005-0.025): 1.
Further; the mass-volume ratio of the absolute ethyl alcohol to the CIP in the step (1) is 10 mL/1 g.
Further; in the step (2), the concentration of the DMAOP is 65wt%, and the mass ratio of the DMAOP to the GO is 1:1.
Further; in the step (4), the mass ratio of VcNa to GO is 1:1, the reduction temperature is 60 ℃, and the reduction time is 2 h.
Further; the multi-element corrosion inhibitor in the step (6) consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1.
Further; the mass ratio of the TPU to the DMF is 0.2:1, the mass ratio of the RGO/CIP composite wave-absorbing material to the TPU is 0.6:1, and the mass ratio of the multi-element corrosion inhibitor to the TPU is 0.15:1.
Further; the ultrasonic treatment in the step (6) is carried out for 30 min, the heating temperature is 60 ℃, and the stirring time is 12 h.
Further; the corrosion inhibition wave absorption integrated film is applied to the fields of corrosion prevention and wave absorption of marine equipment and facility surfaces.
The invention has the beneficial effects that the graphene with dielectric loss behavior and the carbonyl iron with magnetic loss behavior are effectively compounded by utilizing the coupling effect of the silane coupling agent, so that the synergistic effect of a system medium-magnetic double mechanism is realized. The existence of carbonyl iron effectively adjusts impedance mismatch of the system caused by high conductivity of graphene, and simultaneously, a large number of heterojunction surfaces formed between the carbonyl iron and the graphene introduce new interface polarization for the system, so that the electromagnetic wave absorption performance of the composite system is remarkably enhanced. The invention prepares the multifunctional film with long-acting corrosion inhibition performance and wave absorption performance by a simple mixed knife coating mode, and the preparation method is simple and convenient to operate. According to the invention, corrosion inhibition and wave absorption integrated films with different thicknesses are used for coating the sandpaper polished smooth steel sheet and then carrying out salt spray test. After 168 h salt spray test, the corrosion rate of the whole steel sheet is below 5%, the corrosion rate rises along with the increase of the film thickness, and when the thickness is 1 mm, the corrosion rate of the film to the steel sheet can reach 99%, and the corrosion inhibition performance is remarkable. The corrosion inhibition and wave absorption integrated film obtained by the invention has the minimum RLmin of-49 dB at 11.87 GHz when the RGO/CIP-2% film thickness is 2.1 mm and the corresponding effective absorption bandwidth when the GO content is increased to 2%f E =8.25 GHz。
Drawings
FIG. 1 is an SEM of a different material (a) an SEM of CIP; (b) (f) SEM images of RGO/CIP composite wave-absorbing materials prepared in examples 1-5 respectively;
FIG. 2 is an SEM image of an RGO/CIP-2% film prepared in example 4, where (a) and (b) are surface features and an enlarged view; (c) and (d) are cross-sectional morphologies and enlarged views; (e) is a surface Fe element profile; (f) is a surface Si element profile;
FIG. 3 is a structural representation of CIP film and corrosion inhibition and wave absorption integrated film prepared in examples 1-5 (a) is XRD pattern; (b) is an infrared spectrogram; (c) is a raman spectrum;
FIG. 4 is a three-dimensional reflection loss plot of CIP film for different materials; (b) three-dimensional reflection loss pattern of RGO/CIP-0.5% film; (c) three-dimensional reflection loss map of RGO/CIP-1% film; (d) three-dimensional reflection loss pattern of RGO/CIP-1.5% film; (e) three-dimensional reflection loss map of RGO/CIP-2% film; (f) three-dimensional reflection loss pattern of RGO/CIP-2.5% film;
FIG. 5 is a graph of the strongest reflection loss and corresponding effective absorption bandwidth of CIP films and corrosion inhibition and wave absorption integrated films prepared in examples 1-5;
FIG. 6 is a graph of various electromagnetic parameters of CIP film and corrosion inhibition and wave absorption integrated films prepared in examples 1 to 5 (a) is the real part of dielectric constantε′The method comprises the steps of carrying out a first treatment on the surface of the (b) Is the imaginary part of dielectric constantε''The method comprises the steps of carrying out a first treatment on the surface of the (c) Is the dielectric loss tangent tanδεThe method comprises the steps of carrying out a first treatment on the surface of the (d) Is the real part of magnetic permeabilityμ′The method comprises the steps of carrying out a first treatment on the surface of the (e) Is the imaginary part of magnetic conductivityμ″The method comprises the steps of carrying out a first treatment on the surface of the (f) Is the permeability tangent tanμ；
FIG. 7 is an impedance matching diagram of different materials (a) is an impedance matching diagram of a CIP film; (b) is an impedance match plot of RGO/CIP-0.5% film; (c) is an impedance match plot of RGO/CIP-1% film; (d) is an impedance match plot of RGO/CIP-1.5% film; (e) is an impedance match plot of RGO/CIP-2% film; (f) is an impedance match plot of RGO/CIP-2.5% film;
FIG. 8 is a graph showing the damping constants of CIP films and corrosion inhibition and wave absorption integrated films prepared in examples 1 to 5;
FIG. 9 is a graph of corrosion of the surface of a coated lower steel sheet with different film thicknesses after 168 h salt spray test (a) is bare steel; (b) is a pure PU film; (c) a steel sheet covered with a film having a thickness of 0.5. 0.5 mm; (d) a steel sheet covered with a film having a thickness of 0.6. 0.6 mm; (e) is a steel sheet covered with a film having a thickness of 0.7. 0.7 mm; (f) a steel sheet covered with a film having a thickness of 0.8. 0.8 mm; (g) is a steel sheet covered with a film having a thickness of 0.9. 0.9 mm; (h) a steel sheet covered with a film having a thickness of 1 mm;
FIG. 10 is a graph showing corrosion and corrosion inhibition rates of steel sheets coated with different film thicknesses after 168 h salt spray test.
Detailed Description
The following examples are intended to illustrate the present invention in further detail. The following examples are only illustrative of the present invention, but the present invention is not limited to these examples. All equivalent changes and modifications within the scope of the present invention should be made. The various materials referred to in the specification are all available from the market.
DMAOP in the present invention is purchased from Shanghai Alasdine Biochemical technologies Co., ltd.
Example 1:
the preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing 0.05g of GO and 10g of CIP in 100 ml absolute ethyl alcohol, wherein the mass content of GO relative to the CIP is 0.5%;
(2) Adding 0.05g of DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at a rotating speed of 800 rpm for 12 h;
(3) Filtering the stirred mixed solution, flushing the mixed solution by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using 0.05g of VcNa, wherein the reduction temperature is 60 ℃ and the reduction time is 2 h;
(5) Performing suction filtration and drying on the reduced RGO/CIP to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding 0.6g RGO/CIP and 0.15g multi-element corrosion inhibitor into 5g DMF and carrying out ultrasonic treatment for 30 min, then adding 1g TPU, and heating and stirring at 60 ℃ for 12 h to fully mix; the multi-element corrosion inhibitor consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1;
(7) The completely and uniformly dispersed solution is coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain the corrosion inhibition and wave absorption integrated film (named RGO/CIP-0.5 percent film).
Example 2:
the preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing 0.1g of GO and 10g of CIP in 100 ml absolute ethyl alcohol, wherein the mass content of GO relative to the CIP is 1%;
(2) Adding 0.1g of DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at a rotating speed of 800 rpm for 12 h;
(3) Filtering the stirred mixed solution, flushing the mixed solution by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using 0.1g of VcNa, wherein the reduction temperature is 60 ℃ and the reduction time is 2 h;
(5) Performing suction filtration and drying on the reduced RGO/CIP to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding 0.6g RGO/CIP and 0.15g multi-element corrosion inhibitor into 5g DMF and carrying out ultrasonic treatment for 30 min, then adding 1g TPU, and heating and stirring at 60 ℃ for 12 h to fully mix; the multi-element corrosion inhibitor consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1;
(7) The completely and uniformly dispersed solution is coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain the corrosion inhibition and wave absorption integrated film (named RGO/CIP-1 percent film).
Example 3:
the preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing 0.15g of GO and 10g of CIP in 100 ml absolute ethyl alcohol, wherein the mass content of GO relative to the CIP is 1.5%;
(2) Adding 0.15g of DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at a rotating speed of 800 rpm for 12 h;
(3) Filtering the stirred mixed solution, flushing the mixed solution by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using 0.15g of VcNa, wherein the reduction temperature is 60 ℃ and the reduction time is 2 h;
(5) Performing suction filtration and drying on the reduced RGO/CIP to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding 0.6g RGO/CIP and 0.15g multi-element corrosion inhibitor into 5g DMF and carrying out ultrasonic treatment for 30 min, then adding 1g TPU, and heating and stirring at 60 ℃ for 12 h to fully mix; the multi-element corrosion inhibitor consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1;
(7) The completely and uniformly dispersed solution is coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain the corrosion inhibition and wave absorption integrated film (named RGO/CIP-1.5 percent film).
Example 4:
the preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing 0.2g of GO and 10g of CIP in 100 ml absolute ethyl alcohol, wherein the mass content of GO relative to the CIP is 2%;
(2) Adding 0.2g of DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at a rotating speed of 800 rpm for 12 h;
(3) Filtering the stirred mixed solution, flushing the mixed solution by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using 0.2g of VcNa, wherein the reduction temperature is 60 ℃ and the reduction time is 2 h;
(5) Performing suction filtration and drying on the reduced RGO/CIP to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding 0.6g RGO/CIP and 0.15g multi-element corrosion inhibitor into 5g DMF and carrying out ultrasonic treatment for 30 min, then adding 1g TPU, and heating and stirring at 60 ℃ for 12 h to fully mix; the multi-element corrosion inhibitor consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1;
(7) The completely and uniformly dispersed solution is coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain the corrosion inhibition and wave absorption integrated film (named RGO/CIP-2 percent film).
Example 5:
the preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing 0.25g of GO and 10g of CIP in 100 ml absolute ethyl alcohol, wherein the mass content of GO relative to the CIP is 2.5%;
(2) Adding 0.25g of DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at a rotating speed of 800 rpm for 12 h;
(3) Filtering the stirred mixed solution, flushing the mixed solution by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) The GO/CIP composite wave-absorbing material is reduced by 0.25g of VcNa, the reduction temperature is 60 ℃, and the reduction time is 2 h;
(5) Performing suction filtration and drying on the reduced RGO/CIP to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding 0.6g RGO/CIP and 0.15g multi-element corrosion inhibitor into 5g DMF and carrying out ultrasonic treatment for 30 min, then adding 1g TPU, and heating and stirring at 60 ℃ for 12 h to fully mix; the multi-element corrosion inhibitor consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to the mass ratio of 1:2:1;
(7) The completely and uniformly dispersed solution is coated on a glass slide, and then dried at 60 ℃ for 24 h to obtain the corrosion inhibition and wave absorption integrated film (named RGO/CIP-2.5 percent film).
Performance measurement
The form and structure of the RGO/CIP composite wave-absorbing material and the corrosion inhibition wave-absorbing integrated film are observed by a field emission scanning electron microscope (FE-SEM, JEOL, JSM-7800F) as shown in figures 1 and 2. And adopting an X-ray diffraction system (XRD, PW1830, philips) of 10-80 degrees under Cu-K alpha radiation to perform structural characterization analysis on the corrosion inhibition and wave absorption integrated film, wherein the structural characterization analysis is shown in (a) of FIG. 3. The structure of the corrosion inhibition and wave absorption integrated film was characterized using Fourier infrared spectroscopy (FTIR Spectrometer; bruker, TENSOR II) as shown in FIG. 3 (b). The structural differences of the corrosion inhibition and wave absorption integrated film were analyzed by 532 nm argon ion laser raman spectroscopy (insia Renishaw), as shown in fig. 3 (c). The corrosion inhibition and wave absorption integrated film is fused and cast into an annular sample with the outer diameter of 7.0 mm and the inner diameter of 3.04 mm, and the complex permeability and the dielectric constant of the corrosion inhibition and wave absorption integrated film are measured by a coaxial method in the frequency range of 1-18 GHz by using a vector network analyzer (AV 3618, CETC). And testing the RL value of the corrosion inhibition and wave absorption integrated film by using an arch method reflectivity testing system. The steel sheet after the sandpaper is polished clean and smooth is wrapped by corrosion inhibition wave-absorbing integrated films with different thicknesses, and is placed in a salt spray testing machine for salt spray testing, the testing time is 168 h, and the electrolyte solution is 3.5 wt% NaCl solution.
The morphology of CIP and RGO/CIP composite wave-absorbing materials prepared in examples 1-5 was observed by SEM, as shown in FIG. 1. Pure CIP is a platelet structure with a size of 4-5 μm. Under the action of the silane coupling agent, the platy CIP is successfully coupled on the graphene sheet, and as the usage amount of the GO and the silane coupling agent is increased, the combination degree of the graphene sheet and the CIP is better and better, and more CIP is coupled on the graphene sheet to form a large number of heterojunction surfaces (shown in (b) - (e) in fig. 1), so that the interface polarization of the material is facilitated, and the wave absorbing performance of the material is improved. However, due to strong van der Waals interactions and high inter-sheet contact resistance between graphene sheets, graphene is prone to irreversible agglomeration or re-stacking, thereby affecting the performance of the material. After the usage amount of GO is further increased, although more CIP is coupled on the graphene sheets under the action of the silane coupling agent with higher concentration, the graphene sheets can be obviously found to start to agglomerate (fig. 1 (f)), which greatly hinders the conduction of electrons and the transfer of charges in the material, weakens the capability of the material for converting and dissipating electromagnetic wave energy, and finally influences the wave absorbing performance of the material.
Further, the surface and the cross section of the corrosion inhibition and wave absorption integrated film prepared in example 4 are observed, as shown in fig. 2. From SEM image, RGO/CIP composite wave-absorbing material is uniformly dispersed on the surface or section of the film, and the phenomena of accumulation, agglomeration and the like are avoided. Meanwhile, the elements on the surface of the film are analyzed and characterized by utilizing EDS, the Si elements on the surface of the film are uniformly distributed and basically coincide with the distribution of Fe elements, and the coupling effect of the silane coupling agent in the composite material can be proved.
The structure of the corrosion inhibition and wave absorption integrated film analyzed by XRD is shown in (a) of figure 3. Distinct CIP characteristic peaks can be observed in the XRD patterns at 44.5 ° and 64.3 °, corresponding to the (110) and (200) crystal planes thereof, respectively, and further weaker broad peaks in the range of 20-25 °, corresponding to small amounts of RGO and overlapping of lower crystallinity PU characteristic peaks, are present. From the infrared spectrum (fig. 3 (b)), 3332 cm can be found -1 、1736 cm -1 、1600 cm -1 、1530 cm -1 Characteristic peaks of PU appear nearby, which respectively correspond to the combined absorption peaks of N-H bending vibration and C-N vibration of the carbamate structure, C-O stretching vibration and N-H bending vibration; 1738 cm -1 、1395 cm -1 、1225 cm -1 1075 and 1075 cm -1 Characteristic peaks of GO appear, wherein part of characteristic peaks overlap with CIP characteristic peaks, signals become strong, and the range is widened. Notably, the corrosion inhibition and wave absorption integrated film is described in 836 and 836 cm −1 Characteristic absorption peaks appear, corresponding to si—c stretching vibrations, the relevant chemical bonds being present only in DMAOP, indicating successful grafting of DMAOP on the graphite flake. In the raman spectrum (fig. 3 (c)), the D band (1345 cm) was clearly observed for all samples −1 ) And G belt (1580 cm) −1 ) Is a strong peak of (I) D /I G The value (D band intensity/G band intensity value) is widely used to evaluate the relative order of graphene-based materials. As can be seen by comparing films with different GO contents, I D /I G Value by valueIncreasing, due to the varying degree of binding between GO and CIP. When the GO content is smaller, the bonding degree between the graphene sheet and CIP is smaller, and the surface of the sheet is free from a large number of defects such as heterojunction surfaces and the like. With the gradual increase of the content of GO and DMAOP, the combination degree between the graphene sheets and CIP is gradually deepened, and CIP with smaller size is coupled on the graphene sheets, so that a large number of defect sites are formed, and the disorder degree of the system is increased, which is favorable for the attenuation of electromagnetic waves in the material.
And calculating the minimum reflection loss of the corrosion inhibition and wave absorption integrated film according to the transmission line theory. The relationship between the microstructure change of the film and the electromagnetic wave absorption performance is studied.
Wherein,Z in as an input impedance of the microwave absorber,Z 0 in the form of a free-space impedance,ε r （ε r =ε'- jε″) Andμ r （μ r ＝ μ′-jμ″) Respectively the permittivity and the permeability are expressed,ffor the frequency of the microwaves,cin order to achieve the light velocity, the light beam is,dis the thickness of the microwave absorber.
As can be seen from fig. 4, the pure CIP film has a minimum RL of-23 dB at 17.12 GHz, poor absorption due to the single absorption loss mechanism of CIP, and limited absorption at 60% content. After the GO is added, the graphene sheets can form a complete conductive network, so that electromagnetic wave energy is promoted to be converted and dissipated in the material. In addition, due to large size difference, a large number of heterogeneous interfaces are formed between CIP and graphene sheets, and new interface polarization is introduced for the system. Therefore, after GO is added, the wave absorbing performance of the system is obviously improved. Corrosion inhibition wave-absorbing integrated film wave-absorbing performance with different GO contents is compared with that of the filmWith the increase of GO, the wave absorbing performance of the system is increased and then reduced, when the GO content is increased to 2%, the RGO/CIP-2% film has minimum RL of 49 dB at 11.87 GHz and thickness of 2.1 mm, and the corresponding effective absorption bandwidthf E =8.25 GHz (see fig. 5). However, further increasing the amount of GO resulted in a decrease in the wave absorbing properties of the system, with RGO/CIP-2.5% films having a minimum RL of-38 dB at 12.31 GHz and a thickness of 2.3, due primarily to agglomerated stacking between graphene sheets.
To further reveal the wave-absorbing characteristics of the film, the relative complex dielectric constant of the film is within the frequency range of 1-18 GHzε r =ε′-jε'') And relative complex permeabilityμ r =μ′-jμ'') As shown in fig. 6. Wherein the real partε'And real partμ′Representing the storage capacity, imaginary part, of electromagnetic wave energyε″And imaginary partμ″Representing the ability to dissipate electromagnetic wave energy,ε″proportional to the conductivity. As can be seen from FIGS. 6 (a) - (b), the real part of the dielectric constant of all samplesε'As the frequency increases, the dielectric constant imaginary part shows a decreasing trend in the whole frequency range and increases as the GO content increases, which indicates that as GO is added, the dielectric loss capability of the system to electromagnetic waves is improved. tan deltaε（tan δε=ε''/ε′) The value is an important parameter for evaluating the dielectric loss capability of a microwave absorbing material to an incident electromagnetic wave. By calculating tan deltaεThe dielectric loss strength of the material to incident electromagnetic waves was evaluated. As shown in FIG. 6 (c), as the GO content increases, the conductive network in the RGO/CIP system gradually forms, tan deltaεAnd thus gradually increases. However, too high tan deltaεThe impedance mismatch of the system can be caused, so that the addition of GO has a certain limit on the improvement of the system wave absorbing performance. At the same time test the real part of magnetic permeability of different systemsμ′Imaginary part of magnetic conductivityμ''Magnetic permeability tangent tan deltaμ（tan δμ=μ''/μ′) As in (d) - (f) of fig. 6.μ″And tan deltaμThe frequency-dependent variation trend of (c) is the same, and a remarkable effect can be observedFormants (multi-resonance behavior) indicate that CIP in the system generates magnetic loss to electromagnetic waves. In addition, comparative tan deltaεAnd tan deltaμThe former is significantly higher than the latter, indicating that the magnetic CIP brings about relatively weak magnetic loss, and absorption attenuation of incident electromagnetic waves is achieved mainly by dielectric loss for RGO/CIP films.
Impedance matching is a key factor in evaluating absorber MA performance, representing the ability of microwaves to enter the absorbing material and convert to thermal energy or dissipate by interference. To better explore the MA performance of these films, the characteristic impedance z= |z was normalized in /Z 0 Evaluation of impedance matching. When the Z ratio approaches 1, almost all incident electromagnetic waves can penetrate the material integrity without microwave reflectivity, exhibiting optimal impedance matching. Typically, the absorber is considered to have a good impedance match when its Z is in the range of 0.8-1.2 (as in FIG. 7). As shown in fig. 7, the two-dimensional mapping of RGO/CIP film Z values shows that the impedance matching of the pure CIP system is poor, the impedance matching performance of the system increases after adding GO, but the impedance matching is not further optimized with increasing GO content. For graphene-based wave-absorbing materials, the impedance matching performance is closely related to the conductivity, and the higher the conductivity is, the larger the dielectric constant difference between the graphene-based wave-absorbing material and an air medium is, and the worse the impedance matching performance is. The addition of small amounts of GO to CIP adjusts the conductivity of the system and thus the impedance matching performance is enhanced, whereas as GO content increases gradually, the conductivity of the system increases gradually and stabilizes at a higher level (in conjunction with fig. 6 (b)), so the impedance matching cannot be further enhanced.
Furthermore, the damping constantαIs another important factor affecting the performance of the material MA, and is obtained by the following formula, which is used for explaining the attenuation capability of the wave-absorbing material to the incident microwave:
wherein,ffor the frequency of the microwaves,cin order to achieve the light velocity, the light beam is,epsilon' and epsilonRespectively the dielectric constantsε r The real part of (2)With the imaginary part of the signal,μ′andμ″respectively magnetic permeabilityμ r Real and imaginary parts of (a) are provided.
Proper impedance matching performance and high attenuation capability give the absorber excellent MA performance. As can be seen from fig. 8, the decay constant of the system gradually increases with increasing GO content, and decreases with a content exceeding 2%. RGO/CIP-2% film has the largest decay constant, which is attributed to the fact that the 2% GO addition forms a relatively perfect conductive path for the system, and stacking agglomeration of graphene sheets does not occur, so that electrons can be transferred more rapidly, and larger conduction loss is generated. In addition, the combination degree of GO and CIP is good under the addition amount, a large amount of effective heterogeneous interfaces are formed between the graphene sheets and the CIP, new interface polarization is introduced for the system, and the attenuation capability of the system to electromagnetic waves is further enhanced. By combining impedance matching of films with different GO contents, the RGO/CIP-2% film system is verified to have the best electromagnetic wave absorption performance, which is consistent with the actual test.
And testing the corrosion inhibition performance of the corrosion inhibition and wave absorption integrated film by a 168 h salt spray experiment. The fully dispersed and homogeneous solution of step (7) of example 4 was knife coated onto glass slides to a thickness of 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, respectively, and then dried 24 h at 60 ℃ to give RGO/CIP-2% films having a thickness of 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, respectively. The steel sheet was wrapped with pure PU film and RGO/CIP-2% film with thickness of 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, respectively, and compared with the corrosion degree of the steel sheet surface under different protection conditions, as shown in FIG. 9, it was found that the bare steel surface without any protection was completely covered with corrosion products, and the corrosion of the steel sheet surface wrapped with PU film without corrosion inhibitor was also serious. After the corrosion inhibition system is added, the surface of the steel sheet protected by the film with the thickness of 0.5 mm and 0.6 mm has slight corrosion phenomenon caused by edges, and scratches under corrosion traces are still clearly visible. As the film thickness increases, the corrosion on the surface of the steel sheet gradually lessens and is consistent with the finish before corrosion. Meanwhile, as the film thickness is increased, the corrosion rate of the steel sheet is obviously reduced, the corrosion inhibition rate is obviously increased, and the corrosion inhibition rate can reach 99% when the thickness is 1 mm (fig. 10). Therefore, the corrosion inhibition and wave absorption integrated film has excellent corrosion inhibition performance.
In conclusion, the corrosion inhibition and wave absorption integrated film with wide frequency band, high microwave absorption efficiency and long-acting corrosion inhibition performance is successfully prepared. From experimental test results, the addition of GO introduces conductive loss into the system, and enriches the loss mechanism of the system. Meanwhile, by means of the coupling effect of the silane coupling agent, a large number of heterogeneous interfaces are generated, so that the interface polarization of the system is obviously enhanced. RGO/CIP-2% film has a minimum RL of-49 dB at 11.87 GHz and a thickness of 2.1 mm, corresponding effective absorption bandwidthf E And can reach 8.25 GHz. In addition, the addition of the multi-element corrosion inhibition system can protect CIP from corrosion, ensure stable wave absorption performance, and simultaneously ensure that the film has excellent corrosion inhibition performance, and the highest corrosion inhibition efficiency can reach 99% under 168 h salt spray test.
The above-described embodiments are merely preferred embodiments of the present invention, and the present invention is not limited in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.
Claims (9)
1. The preparation method of the corrosion inhibition and wave absorption integrated film is characterized by comprising the following steps of:
(1) Uniformly dispersing GO and CIP in absolute ethyl alcohol;
(2) Adding DMAOP to the mixed solution in the step (1), and then fully stirring the mixed solution at 800 rpm for 12 h;
(3) Carrying out suction filtration on the mixed solution after stirring in the step (2), flushing by using absolute ethyl alcohol during the process, and then carrying out vacuum drying to obtain the GO/CIP composite wave-absorbing material;
(4) Reducing the GO/CIP composite wave-absorbing material by using VcNa;
(5) Performing suction filtration and drying on the reduced GO/CIP composite wave-absorbing material to obtain an RGO/CIP composite wave-absorbing material;
(6) Adding RGO/CIP composite wave-absorbing material and multi-element corrosion inhibitor into DMF, adding TPU after ultrasonic treatment, heating and stirring to fully and uniformly disperse;
(7) The solution which is uniformly dispersed is coated on a glass slide by scraping, and then is dried for 24 h under the condition of 60 ℃ to obtain the corrosion inhibition wave-absorbing integrated film.
2. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the mass ratio of GO to CIP in the step (1) is (0.005-0.025): 1.
3. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the mass-volume ratio of the absolute ethyl alcohol to the CIP in the step (1) is 10 mL/1 g.
4. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein in the step (2), the concentration of the DMAOP is 65wt%, and the mass ratio of the DMAOP to the GO is 1:1.
5. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the mass ratio of VcNa to GO in the step (4) is 1:1, the reduction temperature is 60 ℃, and the reduction time is 2 h.
6. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the multi-element corrosion inhibitor in the step (6) consists of cyclohexylamine carbonate, sodium benzoate and sodium gluconate according to a mass ratio of 1:2:1.
7. The method for preparing the corrosion and wave-absorbing integrated film according to claim 6, wherein the mass ratio of the TPU to the DMF is 0.2:1, the mass ratio of the RGO/CIP composite wave-absorbing material to the TPU is 0.6:1, and the mass ratio of the multi-element corrosion inhibitor to the TPU is 0.15:1.
8. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the ultrasonic time in the step (6) is 30 min, the heating temperature is 60 ℃, and the stirring time is 12 h.
9. The method for preparing the corrosion inhibition and wave absorption integrated film according to claim 1, wherein the corrosion inhibition and wave absorption integrated film is applied to the fields of marine equipment and facility surface corrosion prevention and wave absorption prevention.
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