CN114149786B - Interface polarization enhanced TiO 2 Preparation method of RGO wave-absorbing material - Google Patents
Interface polarization enhanced TiO 2 Preparation method of RGO wave-absorbing material Download PDFInfo
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Abstract
The invention provides interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material comprises the following steps ofThe method comprises the following steps: step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution; step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state; step 3, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite; step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite. The invention uses hydrogen atmosphere heat treatment to treat TiO 2 An amorphous interface layer with nanoscale thickness is formed on the surface of the nanoparticle to form a nano heterogeneous interface, so that the dielectric loss performance of the nanoparticle is remarkably 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 TiO 2 A preparation method of RGO wave-absorbing material.
Background
With the wide application of wireless communication devices, electromagnetic pollution is generated more and more seriously, which seriously affects communication, equipment safety and human health, and becomes an important problem to be solved. A wave-absorbing material is a material that is capable of converting electromagnetic energy into other forms of energy, reducing reflection of electromagnetic energy. The electromagnetic wave absorbing material has the performance requirements of strong absorbing capacity, wide absorbing frequency band, thin thickness, low density, stable performance and the like. Conventional wave absorbing materials such as ferrite and carbon-based wave absorbing agents have been difficult to meet the stringent requirements imposed by current applications.
The wave-absorbing materials can be classified into three types of magnetic loss, electric conduction loss and dielectric loss according to 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 hysteresis loss of the magnetic material. Typical magnetically lossy materials are: fe. Ni and alloy powder thereof, carbonyl iron and the like have strong magnetic loss capability, and the wave absorbing performance is influenced by the microstructure and content of the material and the impedance matching characteristic of the material. However, the density of the magnetic material is generally larger, the stability is generally higher, the skin effect is obvious, the response frequency is limited, and the magnetic loss in the high-frequency GHz frequency band is obviously reduced, so that the practical application of the magnetic material in the field of wave-absorbing materials, especially in the X-band, is restricted. The electrically conductive lossy wave-absorbing material attenuates electromagnetic waves by the interaction of carriers with an electric field. Typical electrically conductive lossy materials such as carbon-based materials, for example: graphite powder, carbon black, carbon fibers, carbon Nanotubes (CNTs), and the like. When (when)The use of front carbon-based wave absorbing materials 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 great difficulty; secondly, because the conductivity of the carbon material is higher, the loss capacity is very strong, a conductive channel is easy to form when the percolation threshold is reached, the impedance matching requirement is often not favorably met, and the high requirement is put forward on the component proportion of the wave absorber. Dielectric loss type wave absorbing materials attenuate electromagnetic wave energy through electron polarization, ion polarization, molecular polarization, dipole polarization and interface polarization, and in high-frequency X-band electromagnetic waves, interface polarization is an important dielectric loss mechanism. Typical dielectric loss materials are: zinc oxide (ZnO), silicon carbide (SiC), titanium oxide (TiO 2 ) Barium titanate (BaTiO) 3 ) Etc. The conductivity of the dielectric loss material is much lower than that of the conductor material, free electrons are hardly generated in the material, macroscopic current is not generated in the material under the action of an external electric field, so impedance mismatch is not generally caused, but the dielectric loss capacity is generally not strong, and a larger filling rate is required to achieve ideal wave absorbing performance, so that the density of the wave absorbing material is not reduced, and the performance is still further optimized.
The single loss mechanism wave absorbing material has the defects of low absorption intensity, narrow absorption frequency band, poor impedance characteristic, high filling ratio and the like, and limits the practical application thereof. By compounding materials with different loss mechanisms, the wave-absorbing material with more excellent performance can be obtained. Therefore, composite wave-absorbing materials are receiving much attention. Kong et al assemble low dielectric loss type cobalt tetrapyridyl porphyrin on the surface of high conductivity loss type multiwall carbon nanotube to form nano heterostructure, enhancing polarization loss of hetero interface, and the composite material has excellent wave absorption performance, and reflection coefficient is less than-50 dB 1 in X wave band. Zhao et al studied the wave absorbing properties of nitrogen (N) doped nano SiC particles, N in the SiC nano grains substituted for C to form element doping, as dielectric loss phase, and combined with graphite conductance loss to form composite wave absorbing material, having lower real part of dielectric constant and higher dielectric loss, and reflection coefficient less than-10 dB < 2 > in 9.8-15.8 GHz. However, not any two materials can be combined to optimize the wave absorbing performance. To obtain excellent wave absorbing performance, the wave absorbing material is required to meet the special requirement of impedance matching, ensure that electromagnetic wave enters the material, and simultaneously has strong loss capability and can fully absorb the incident electromagnetic wave energy. Therefore, aiming at the electromagnetic pollution of the high-frequency X-band, the synergy of strong electromagnetic loss and impedance matching is a key scientific difficulty faced by developing a novel wave-absorbing material, and a wave-absorbing material which can meet the impedance matching requirement and has strong interface polarization and dielectric loss capacity is urgently required.
Disclosure of Invention
The invention aims to provide interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material can prepare the wave-absorbing material with strong conductivity and conductivity loss capacity.
The invention adopts the technical proposal that the interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
step 3, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite.
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 uniform mixed solution is 0.1-0.3 mol/L.
And 2, uniformly mixing the solution in the step, wherein the reaction temperature in the polytetrafluoroethylene lining autoclave is 140-180 ℃ and the reaction time is 4-10 h.
In the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
In the step 4, the reducing gas is one of hydrogen/argon or a mixed gas of hydrogen/nitrogen.
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 beneficial effects of the invention are as follows:
1) The invention relates to interface polarization enhancement type TiO 2 Preparation method of RGO wave-absorbing material, which adopts liquid phase method to combine two-dimensional nano GO sheet layer with TiO 2 The precursor is uniformly distributed on a microscopic scale, and the GO surface has a large number of groups, so the catalyst is suitable for being used as a carrier and TiO 2 The nanoparticles are composited. The TiO obtained 2 TiO in RGO wave-absorbing composite material 2 The nano particles are uniformly distributed on the surface of the two-dimensional nano RGO sheet layer.
2) Interface enhanced TiO prepared by the invention 2 RGO wave-absorbing composite material is prepared by heat treatment in hydrogen atmosphere on TiO 2 An amorphous interface layer with nanoscale thickness is formed on the surface of the nanoparticle to form a nano heterogeneous interface, so that the dielectric loss performance of the nanoparticle is remarkably enhanced.
3) Interface enhanced TiO prepared by the invention 2 According to the RGO wave-absorbing composite material, GO is converted into RGO through hydrogen treatment, and the conductivity loss capacity are remarkably improved.
4) Interface enhanced TiO prepared by the invention 2 RGO wave-absorbing composite material prepared by adjusting TiO 2 Dielectric constant and dielectric loss of RGO two-phase proportion adjustable composite material, and prepared TiO 2 The RGO wave-absorbing composite material has controllable dielectric loss performance.
Drawings
FIG. 1 is a TiO of example 1 of the present invention 2 Low-power transmission electron microscope photo of RGO wave absorbing material;
FIG. 2 is a TiO of example 1 of the present invention 2 High-power transmission electron microscope photo of/RGO wave-absorbing material
FIG. 3 is a TiO of example 1 of the present invention 2 RGO absorberXRD spectrum of the wave material;
FIG. 4 is a TiO of example 1 of the present invention 2 Raman spectrogram of RGO wave-absorbing material;
FIG. 5 is a TiO of example 1 of the present invention 2 Dielectric property curve of RGO wave-absorbing material;
FIG. 6 is a TiO according to example 4 of the present invention 2 Dielectric properties curves of/RGO absorbing materials.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention provides interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
the volume ratio of the ethanol to the water in the mixed solution of the ethanol and the water is 10:1, the GO content is 0.05-0.2 mg/mL, and the molar concentration of the tetrabutyl titanate in the uniform mixed solution is 0.1-0.3 mol/L.
Step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
the reaction temperature of the uniform mixed solution in the polytetrafluoroethylene lining autoclave is 140-180 ℃ and the reaction time is 4-10 h.
Step 3, collecting a solid phase product through centrifugation, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
in the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
Step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
the reducing gas is one of hydrogen/argon or mixed gas of hydrogen/nitrogen, the volume fraction content of the hydrogen in the reducing gas is 5-20%, the heat treatment temperature is 500-700 ℃, and the heat treatment time is 1-5 h.
Heat treatment of TiO by hydrogen atmosphere 2 An amorphous interface layer with nanoscale thickness is formed on the surface of the nanoparticle, a nano heterogeneous interface is formed, the dielectric loss performance of the nano heterogeneous interface is remarkably enhanced, GO is converted into RGO through hydrogen treatment, and the conductivity loss capability are remarkably improved. By compounding the conductive loss type RGO and the dielectric loss type TiO2, better wave absorbing performance can be achieved when the content of the wave absorbing agent is low, and therefore high-efficiency wave absorbing performance is achieved.
Example 1
Interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
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 0.1mol/L.
Step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene-lined autoclave was 140 ℃ and the reaction time was 4 hours.
Step 3, collecting a solid phase product through centrifugation, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
in the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
Step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
the reducing gas is one of hydrogen/argon or mixed gas of hydrogen/nitrogen, the volume fraction content of the hydrogen in the reducing gas is 5 percent, the heat treatment temperature is 500 ℃, and the heat treatment time is 1h.
Example 2
Interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
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 uniform mixed solution is 0.2mol/L.
Step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene lining autoclave is 150 ℃ and the reaction time is 6 hours.
Step 3, collecting a solid phase product through centrifugation, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
in the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
Step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
the reducing gas is one of hydrogen/argon or mixed gas of hydrogen/nitrogen, the volume fraction content of the hydrogen in the reducing gas is 10 percent, the heat treatment temperature is 600 ℃, and the heat treatment time is 4 hours.
Example 3
Interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
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 0.25mol/L.
Step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene lining autoclave is 160 ℃ and the reaction time is 8 hours.
Step 3, collecting a solid phase product through centrifugation, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
in the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
Step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
the reducing gas is one of hydrogen/argon or mixed gas of hydrogen/nitrogen, the volume fraction content of the hydrogen in the reducing gas is 15 percent, the heat treatment temperature is 600 ℃, and the heat treatment time is 8 hours.
Example 4
Interface polarization enhanced TiO 2 The preparation method of the RGO wave-absorbing material is specifically implemented according to the following steps:
step 1, dispersing GO in a mixed solution of ethanol and water through ultrasonic treatment to obtain GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
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 0.3mol/L.
Step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
the reaction temperature of the uniformly mixed solution in the polytetrafluoroethylene lining autoclave is 180 ℃ and the reaction time is 10 hours.
Step 3, collecting a solid phase product through centrifugation, washing the solid phase product sequentially by ethanol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
in the step 3, the solid phase products are respectively washed in absolute ethanol and water for 5min.
Step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
the reducing gas is one of hydrogen/argon or mixed gas of hydrogen/nitrogen, the volume fraction content of the hydrogen in the reducing gas is 20 percent, the heat treatment temperature is 700 ℃, and the heat treatment time is 5 hours.
FIGS. 1-2 are diagrams of TiO prepared in example 1 2 Transmission electron microscopy of RGO nanocomposite, from which TiO can be seen 2 The particle diameter of the nano particles is about 30nm, the particle diameter is uniformly distributed, and the TiO is prepared 2 The nano particles are uniformly loaded on the RGO surface, and TiO can be observed from a high-resolution transmission electron microscope image 2 The surface of the nanoparticle has an amorphous interface layer approximately 1 nm thick.
FIG. 3 is a TiO film prepared in example 1 2 XRD spectrum of RGO wave-absorbing material, diffraction peak and TiO in the graph 2 In line, no obvious carbon diffraction peak appears in the figure due to the low RGO content in the composite material.
FIG. 4 is a TiO film prepared in example 1 2 Raman spectra of RGO absorbing materials, typical D band and G band of carbon materials can be observed, while TiO 2 The Raman response of (c) is weaker and a weaker characteristic peak appears at low wavenumbers.
FIG. 5 is a TiO prepared in example 1 2 The dielectric performance 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 is a TiO prepared in example 4 2 The 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 and the imaginary part is between3.6-4.2, the loss tangent is approximately equal to 0.4, the dielectric loss capacity is moderate, the impedance matching requirement is favorably met, and the wave absorbing performance is better
Through the mode, the interface polarization enhanced TiO of the invention 2 The wave-absorbing material prepared by the preparation method of the RGO wave-absorbing material is prepared in TiO by hydrogen atmosphere heat treatment 2 An amorphous interface layer with nanoscale thickness is formed on the surface of the nanoparticle, a nano heterogeneous interface is formed, the dielectric loss performance of the nano heterogeneous interface is remarkably enhanced, GO is converted into RGO through hydrogen treatment, and the conductivity loss capability are remarkably improved. By compounding the conductive loss type RGO and the dielectric loss type TiO2, better wave absorbing performance can be achieved when the content of the wave absorbing agent is low, and therefore high-efficiency wave absorbing performance is achieved.
Claims (4)
1. Interface polarization enhanced TiO 2 The 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 GO suspension, then adding a mixed solution of tetrabutyl titanate and ethanol, and magnetically stirring to obtain a uniform mixed solution;
step 2, placing the uniform mixed solution obtained in the step 1 into a polytetrafluoroethylene lining autoclave, and preparing a solid-phase product at a high temperature state;
step 3, washing the solid phase product sequentially by absolute ethyl alcohol and water, and then drying in vacuum to obtain TiO 2 GO nanocomposite;
step 4, tiO 2 Placing the GO nanocomposite in a tube furnace, and introducing reducing gas into the tube furnace for heat treatment to obtain the composite;
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 uniform mixed solution is 0.1-0.3 mol/L;
and (2) the reaction temperature of the uniformly mixed solution in the step (2) in the polytetrafluoroethylene lining autoclave is 140-180 ℃ and the reaction time is 4-10 h.
2. The interface polarization-enhanced TiO according to claim 1 2 The 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 5min.
3. The interface polarization-enhanced TiO according to claim 1 2 The 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.
4. The interface polarization-enhanced TiO according to claim 1 2 The 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 5-20%, the heat treatment temperature is 500-700 ℃, and the heat treatment time is 1-5 h.
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