CN114149786A - Interface polarization enhanced TiO2Preparation method of/RGO wave-absorbing material - Google Patents
Interface polarization enhanced TiO2Preparation method of/RGO wave-absorbing material Download PDFInfo
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Abstract
The present invention provides an interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps: step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain a GO suspension, adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution; step 2, putting the uniformly mixed solution obtained in the step 1 into a polytetrafluoroethylene lining high-pressure kettle, and preparing a solid-phase product at a high temperature; step 3, washing the solid-phase product with ethanol and water in turn, and then drying in vacuum to obtain TiO2a/GO nanocomposite; step 4, adding TiO2And placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material. The invention adopts hydrogen atmosphere heat treatment to prepare TiO2An amorphous interface layer with nano-scale thickness is formed on the surface of the nano-particles to form a nano-heterogeneous interface, so that the dielectric loss performance of the nano-particles is obviously enhanced.
Description
Technical Field
The invention belongs to the technical field of preparation methods of wave-absorbing materials, and particularly relates to interface polarization enhanced TiO2A preparation method of/RGO wave-absorbing material.
Background
With the wide application of wireless communication equipment, the electromagnetic pollution generated along with the wireless communication equipment is more serious, which seriously affects the communication, equipment safety and human health, and becomes an important problem to be solved urgently. The wave-absorbing material is a material capable of converting electromagnetic wave energy into energy in other forms and reducing electromagnetic energy reflection. The electromagnetic wave absorbing material should have the performance requirements of strong absorption capacity, wide absorption frequency band, thin thickness, low density, stable performance and the like. The traditional wave-absorbing materials such as ferrite, carbon-based wave-absorbing agent and the like are difficult to meet the harsh requirements of current application.
The wave-absorbing material can be divided into three types of magnetic loss, conductive loss and dielectric loss according to a wave-absorbing mechanism. The attenuation loss of the magnetic loss type wave-absorbing material to electromagnetic waves mainly comes from resonance, eddy current loss and magnetic hysteresis loss of the magnetic material. Typical magnetically lossy materials are: fe. Ni and its alloy powder, carbonyl iron, etc. have strong magnetic loss capability, and its wave-absorbing property is influenced by microstructure and content of material and impedance matching property of material. However, the magnetic material has the advantages of generally high density, general stability, obvious skin effect, limited response frequency and obviously reduced magnetic loss in a high-frequency GHz band, so that the practical application of the magnetic material in the field of wave-absorbing materials, particularly X wave bands, is restricted. The conductive loss type wave-absorbing material attenuates electromagnetic waves through the interaction of carriers and an electric field. Typical electrically conductive lossy materials are carbon-based materials such as: graphite powder, carbon black, carbon fibers, Carbon Nanotubes (CNTs), and the like. The application of the current carbon-based wave-absorbing material faces several problems: firstly, carbon nano wave-absorbing materials such as CNTs are easy to agglomerate, and the dispersion of the carbon nano wave-absorbing materials in a matrix is a difficult problem; secondly, the carbon material has high conductivity and high loss capacity, so that a conductive channel is easy to form when the percolation threshold is reached, the requirement of impedance matching is not easily met, and the high requirement is provided for the component proportion of the absorber. The dielectric loss type wave-absorbing material attenuates electromagnetic wave energy through electronic polarization, ion polarization, molecular polarization, dipole polarization and interface polarization, and the interface polarization is an important dielectric loss mechanism in high-frequency X-band electromagnetic waves. Typical dielectric loss materials are: zinc oxide (ZnO), silicon carbide (SiC), titanium oxide (TiO)2) Barium titanate (BaTiO)3) And the like. The conductivity of the dielectric loss material is much lower than that of a conductor material, almost no free electrons exist in the material, and no macroscopic current can be formed in the material under the action of an external electric field, so that impedance mismatch generally cannot be caused, but the dielectric loss capacity is generally not strong, the ideal wave-absorbing performance can be achieved only by needing a larger filling rate, the density of the wave-absorbing material is not reduced favorably, and the performance has a further optimized space.
The single loss mechanism wave-absorbing material has the defects of low absorption strength, narrow absorption frequency band, poor impedance characteristic, high filling proportion and the like, and the practical application of the material is limited. By compounding different loss mechanism materials, the wave-absorbing material with more excellent performance can be obtained. Therefore, the composite wave-absorbing material is widely concerned. Kong et al assemble low dielectric loss type cobalt tetrapyridyl porphyrin on the surface of high conductivity loss type multi-walled carbon nanotube to form a nano heterostructure, which enhances the polarization loss of the heterostructure interface, and the composite material obtains excellent wave absorbing performance with a reflection coefficient less than-50 dB 1 in the X wave band. Zhao et al have studied the wave-absorbing performance of nitrogen (N) element doped nano SiC particles, N element in SiC nano crystal grain replaces C element to form element doping as dielectric loss phase, and combines with graphite conduction loss to form composite wave-absorbing material, which has lower real part of dielectric constant and higher dielectric loss, and the reflection coefficient is less than-10 dB < 2 > in 9.8-15.8 GHz. However, the wave-absorbing properties may not be optimized by compounding any two materials. To obtain excellent wave-absorbing performance, the wave-absorbing material needs to meet the specific requirement of impedance matching to ensure that electromagnetic waves can enter the material, and simultaneously needs to have strong loss capacity to fully absorb the energy of the incident electromagnetic waves. Therefore, aiming at high-frequency X-band electromagnetic pollution, the synergy of strong electromagnetic loss and impedance matching is a key scientific problem for developing novel wave-absorbing materials, and a wave-absorbing material which can meet the impedance matching requirement and has strong interface polarization and dielectric loss capacity is urgently needed to be sought.
Disclosure of Invention
The invention aims to provide interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material can prepare the wave-absorbing material with strong conductivity and conductivity loss capability.
The technical scheme adopted by the invention is that the interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
step 4, adding TiO2And placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material.
The invention is also characterized in that:
in the step 1, the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.05-0.2 mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.1-0.3 mol/L.
And (3) in the step (2), the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene lining autoclave is 140-180 ℃, and the reaction time is 4-10 h.
And in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
In the step 4, the reducing gas is one of hydrogen/argon gas or mixed gas of hydrogen/nitrogen gas.
In the step 4, the volume fraction content of hydrogen in the reducing gas is 5-20%, the heat treatment temperature is 500-700 ℃, and the heat treatment time is 1-5 h.
The invention has the beneficial effects that:
1) the invention relates to interface polarization enhanced TiO2A preparation method of/RGO wave-absorbing material comprises the step of adopting a liquid phase method to combine a two-dimensional nano GO sheet layer with TiO2The precursor is uniformly distributed on a micro scale, and a large number of groups are arranged on the GO surface, so that the GO is suitable for being used as a carrier and TiO2And (4) compounding the nano particles. Obtained TiO2TiO in/RGO wave-absorbing composite material2The nano particles are uniformly distributed on the surface of the two-dimensional nano RGO sheet layer.
2) The interface enhanced TiO prepared by the invention2the/RGO wave-absorbing composite material is prepared by performing heat treatment on TiO in hydrogen atmosphere2A layer of amorphous interface layer with nano-scale thickness is formed on the surface of the nano-particles to form a nano-heterogeneous interface, which is remarkableEnhance the dielectric loss performance.
3) The interface enhanced TiO prepared by the invention2the/RGO wave-absorbing composite material is characterized in that GO is converted into RGO through hydrogen treatment, and the conductivity loss capability are remarkably improved.
4) The interface enhanced TiO prepared by the invention2/RGO wave-absorbing composite material prepared by adjusting TiO2RGO two-phase ratio controllable composite material dielectric constant and dielectric loss, prepared TiO2the/RGO wave-absorbing composite material has controllable dielectric loss performance.
Drawings
FIG. 1 shows TiO prepared in example 1 of the present invention2A low-power transmission electron microscope photo of the/RGO wave absorbing material;
FIG. 2 shows TiO prepared in example 1 of the present invention2High-power transmission electron microscope photo of/RGO wave absorbing material
FIG. 3 shows TiO prepared in example 1 of the present invention2XRD spectrogram of/RGO wave-absorbing material;
FIG. 4 shows TiO prepared in example 1 of the present invention2Raman spectrogram of/RGO wave-absorbing material;
FIG. 5 shows TiO prepared in example 1 of the present invention2Dielectric property curve of/RGO wave-absorbing material;
FIG. 6 shows TiO prepared in example 4 of the present invention2Dielectric property curve of/RGO wave-absorbing material.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The present invention provides an interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.05-0.2 mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.1-0.3 mol/L.
the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene lining autoclave is 140-180 ℃, and the reaction time is 4-10 h.
and in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
Step 4, adding TiO2Placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material;
the reducing gas is one of hydrogen/argon gas or hydrogen/nitrogen gas mixture, the volume fraction content of hydrogen in the reducing gas is 5-20%, the heat treatment temperature is 500-700 ℃, and the heat treatment time is 1-5 h.
By heat treatment in a hydrogen atmosphere on TiO2A layer of amorphous interface layer with nano-scale thickness is formed on the surface of the nano-particles to form a nano heterogeneous interface, so that the dielectric loss performance of the nano-particles is obviously enhanced, GO is converted into RGO through hydrogen treatment, and the conductivity loss capability are obviously improved. By compounding the conductivity loss type RGO and the dielectric loss type TiO2, the wave absorbing agent can achieve better wave absorbing performance at lower wave absorbing agent content, thereby realizing high-efficiency wave absorbing performance.
Example 1
Interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.05mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.1 mol/L.
the reaction temperature of the uniformly mixed solution in a polytetrafluoroethylene lining autoclave is 140 ℃, and the reaction time is 4 h.
and in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
Step 4, adding TiO2Placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material;
the reducing gas is one of hydrogen/argon gas or hydrogen/nitrogen gas mixture, the hydrogen volume fraction content in the reducing gas is 5%, the heat treatment temperature is 500 ℃, and the heat treatment time is 1 h.
Example 2
Interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.1mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.2 mol/L.
the reaction temperature of the uniformly mixed solution in a polytetrafluoroethylene lining autoclave is 150 ℃, and the reaction time is 6 h.
and in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
Step 4, adding TiO2Placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material;
the reducing gas is one of hydrogen/argon gas or hydrogen/nitrogen gas mixture, the hydrogen volume fraction content in the reducing gas is 10%, the heat treatment temperature is 600 ℃, and the heat treatment time is 4 hours.
Example 3
Interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.15mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.25 mol/L.
the reaction temperature of the uniformly mixed solution in a polytetrafluoroethylene lining autoclave is 160 ℃, and the reaction time is 8 h.
and in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
Step 4, adding TiO2Placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material;
the reducing gas is one of hydrogen/argon gas or hydrogen/nitrogen gas mixture, the volume fraction content of the hydrogen in the reducing gas is 15%, the heat treatment temperature is 600 ℃, and the heat treatment time is 8 hours.
Example 4
Interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is implemented according to the following steps:
the volume ratio of ethanol to water in the mixed solution of ethanol and water is 10:1, the GO content is 0.2mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.3 mol/L.
the reaction temperature of the uniformly mixed solution in a polytetrafluoroethylene lining autoclave is 180 ℃, and the reaction time is 10 h.
and in the step 3, the solid-phase product is washed in absolute ethyl alcohol and water for 5min respectively.
Step 4, adding TiO2Placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material;
the reducing gas is one of hydrogen/argon gas or hydrogen/nitrogen gas mixture, the volume fraction content of the hydrogen in the reducing gas is 20%, the heat treatment temperature is 700 ℃, and the heat treatment time is 5 hours.
FIGS. 1-2 show TiO prepared in example 12Transmission electron microscope picture of/RGO nano composite material, from which TiO can be seen2The particle size of the nano-particles is about 30nm, the particle size distribution is uniform, and TiO2The nano particles are uniformly loaded on the RGO surface, and TiO can be observed from a high-resolution transmission electron microscope picture2The surface of the nano-particles is provided with an amorphous interface layer with the thickness close to 1 nanometer.
FIG. 3 shows TiO prepared in example 12XRD spectrogram of/RGO wave-absorbing material, diffraction peak and TiO in the diagram2In line, no significant carbon diffraction peaks appear in the figure due to the low RGO content in the composite.
FIG. 4 shows TiO prepared in example 12The Raman spectrogram of the/RGO wave-absorbing material can observe the D band and the G band which are typical of carbon materials, while TiO can be observed2The Raman response of the compound is weaker, and a weaker characteristic peak appears at a low wave number.
FIG. 5 shows TiO prepared in example 12The dielectric property diagram of the/RGO wave-absorbing material shows that the real part of the dielectric constant is between 5.2 and 5.5, the imaginary part is between 0.7 and 0.9, the loss tangent is less than 0.2, and the dielectric loss capacity is weaker.
FIG. 6 shows TiO prepared in example 42The dielectric property diagram of the/RGO wave-absorbing material shows that the real part of the dielectric constant is between 10.3 and 11.1, the imaginary part is between 3.6 and 4.2, the loss tangent is approximately equal to 0.4, the dielectric loss capacity is moderate, the impedance matching requirement can be favorably met, the wave-absorbing property is better
By the mode, the interface polarization enhanced TiO disclosed by the invention2The wave-absorbing material prepared by the preparation method of the/RGO wave-absorbing material is subjected to heat treatment in a hydrogen atmosphere on TiO2A layer of amorphous interface layer with nano-scale thickness is formed on the surface of the nano-particles to form a nano heterogeneous interface, so that the dielectric loss performance of the nano-particles is obviously enhanced, GO is converted into RGO through hydrogen treatment, and the conductivity loss capability are obviously improved. By compounding the conductivity loss type RGO and the dielectric loss type TiO2, the wave absorbing agent can achieve better wave absorbing performance at lower wave absorbing agent content, thereby realizing high-efficiency wave absorbing performance.
Claims (6)
1. Interface polarization enhanced TiO2The preparation method of the/RGO wave-absorbing material is characterized by comprising the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain a GO suspension, adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
step 2, putting the uniformly mixed solution obtained in the step 1 into a polytetrafluoroethylene lining high-pressure kettle, and preparing a solid-phase product at a high temperature;
step 3, washing the solid-phase product with absolute ethyl alcohol and water in sequence, and then drying in vacuum to obtain TiO2a/GO nanocomposite;
step 4, adding TiO2And placing the/GO nano composite material in a tubular furnace, and introducing reducing gas into the tubular furnace for heat treatment to obtain the composite material.
2. The interfacial polarization enhanced TiO of claim 12The preparation method of the/RGO wave-absorbing material is characterized in that the volume ratio of ethanol to water in the mixed solution of ethanol and water in the step 1 is 10:1, the GO content is 0.05-0.2 mg/mL, and the molar concentration of tetrabutyl titanate in the uniformly mixed solution is 0.1-0.3 mol/L.
3. The interfacial polarization enhanced TiO of claim 12The preparation method of the/RGO wave-absorbing material is characterized in that the reaction temperature of the uniformly mixed solution in the step 2 in a polytetrafluoroethylene lining high-pressure kettle is 140-180 ℃, and the reaction time is 4-10 hours.
4. The interfacial polarization enhanced TiO of claim 12The preparation method of the/RGO wave-absorbing material is characterized in that the solid-phase product in the step 3 is respectively washed in absolute ethyl alcohol and water for 5 min.
5. The interfacial polarization enhanced TiO of claim 12The preparation method of the/RGO wave-absorbing material is characterized in that the reducing gas in the step 4 is one of hydrogen/argon or mixed gas of hydrogen/nitrogen.
6. The interfacial polarization enhanced TiO of claim 12The preparation method of the/RGO wave-absorbing material is characterized in that the volume fraction content of hydrogen in the reducing gas in the step 4 is 5 to20%, the heat treatment temperature is 500-700 ℃, and the heat treatment time is 1-5 h.
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| CN116322008A (en) * | 2023-02-23 | 2023-06-23 | 之江实验室 | Hollow-structure rGO wave-absorbing material and preparation method and application thereof |
| CN116322007A (en) * | 2023-02-23 | 2023-06-23 | 之江实验室 | NiFe-CNTs-RGO composite aerogel material with three-dimensional interconnected pore structure, and preparation method and application thereof |
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