CN110581429B - Terahertz wave radiation source based on graphene material - Google Patents
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Abstract
The invention discloses a terahertz wave radiation source based on a graphene material, relates to a terahertz emission source, and belongs to the technical field of terahertz waves. The basic main body material is graphene and a modified graphene material thereof, and the main structure mainly comprises a semiconductor base layer constructed by graphene and the modified graphene material thereof, a transition transmission interaction layer formed by a transition metal compound, and a graphene magnetic field emission layer formed by graphene and a composite material thereof. The invention provides a real terahertz wave source, the output frequency completely covers the range of 0.1-10 THz terahertz waves, and the terahertz waves with the average power of several milliwatts can be emitted even under the voltage of 24V direct current. The invention has the advantages of simple structure, portability, high film-forming degree, wide working range and high conversion efficiency far exceeding that of the existing terahertz wave radiation source, is completely suitable for mass production and application, and has profound influence on the development of cognitive dimension and depth in the fields of spectroscopy, materials science, biology, medical imaging, environmental science, information science, astrophysics, plasma physics and the like.
Description
Technical Field
The invention belongs to the technical field of terahertz waves, and particularly relates to a novel terahertz radiation source based on graphene and a graphene composite material thereof.
Background
Terahertz waves (THz), also known as T-rays (T-rays), are electromagnetic radiation between millimeter waves and infrared rays with a frequency in the range of 0.1 to 10THz (wavelength 30 μm to 3 mm), are the leading-edge field of technology in electromagnetic spectroscopy research at present, and are also a band that is hardly developed. In recent years, with the progress and intensive research of scientific technology, it is found that due to the special position of the spectrum of the terahertz wave, the optical properties of the spectrum, such as emission, reflection, transmission and the like, contain abundant physical and chemical information, and the terahertz wave can be used as a complementary tool of a Fourier transform infrared spectrum technology and an X-ray technology, is particularly more important for the development of novel fields, such as semiconductors, plasmas, biological materials and the like, and meets special requirements.
Terahertz waves have several unique properties in addition to the properties of electromagnetic waves. The terahertz wave band has the characteristics of coherence, low energy, selectivity, high penetrability and the like, and the characteristics endow huge potential in the basic field and other special fields. In the aspects of medical diagnosis and biotechnology, as the vibration frequency and the rotation energy level of a plurality of biomacromolecules are positioned in the terahertz wave energy wave band, the terahertz wave technology can be utilized to obtain abundant physical and chemical characteristic information fingerprint spectrums, and real biological substance information can be obtained, thus the method can be used for obtaining the biological substance informationMainly because the terahertz wave photon energy is only one part per million (1/10) of the X-ray energy 6 ) Can not cause ionization injury of organisms. Based on the high selectivity and low energy, the irreplaceable advantages of the terahertz waves in biological research, life science and medicine are established. .
The terahertz has strong penetrating power, can detect metal and dangerous objects such as nonmetal, colloid, powder, ceramic, liquid and the like carried by a human body and can be systematically identified, can be used as a safe human body inspection technology, can realize the detection of forbidden safety objects such as smuggled drugs, guns, explosives and the like, can be well applied to the fields of airports, high-speed rails, frontier defense and the like, and has great significance for ensuring the safety of public society and maintaining the stability of national defense. The terahertz is provided with the 'wall-through technology' which can detect weapons hidden behind walls, disguise buried personnel, display equipment such as tanks and artillery in sand dust or smoke, detect underground mine field plastic bombs, fluid explosives, human bombs and the like, and greatly improve the fighting capacity of combat troops and the roadway fighting capacity of troops. In addition, the terahertz wave has the advantages of large communication transmission quantity, high domain frequency spectrum signal-to-noise ratio and high safety, is several times or even thousands times faster than the current ultra-wideband technology, determines the development level of the fields of high-precision secret communication, inter-satellite broadband communication, radar and the like, and influences national defense and military strength. Recent reports also indicate that the terahertz wave is more time-efficient, non-contact and accurate in qualitative and quantitative analysis of other air pollutants such as PM 2.5. Because of the huge development potential and uniqueness, the 2004-year terahertz wave is evaluated as one of ten major technologies for changing the future world in the united states, and is listed as the first major strategic target of national pillars in japan in 2005, and corresponding research and development are vigorously carried out. Terahertz waves have been developed as one of the most important emerging subjects, and the development of the terahertz waves must further restrict the comprehensive strength of national science and technology and the quality of national life. In addition, the method has wide application prospect and academic value in the fields of astrophysics, plasma physics, spectroscopy, materials science, biology, medical imaging, environmental science, information science and the like. At present, the research on terahertz wave technology is gradually developed in China, and corresponding subjects are more and more comprehensive, but most of the subjects are still in the initial starting stage.
Currently, the terahertz wave research technology mainly includes research on a terahertz wave generating source and a detection element thereof, physical and chemical characterization of a terahertz wave band, terahertz wave imaging, and the like. As is well known, the generation, regulation and measurement of terahertz waves in terahertz wave technology are very difficult, wherein the biggest barrier is to obtain terahertz wave radiation with high flux, high stability, high output power and low cost. Terahertz wave bands are related to electronic and optical properties, and corresponding generation sources can also be derived from both methods. Electronic methods are mainly used to up-convert millimeter waves to terahertz waves, for example: common Backward Wave Oscillators (BWO) can produce coherent output with continuously tuned frequency in the sub-terahertz region, but when the frequency exceeds 1THz, the output power and operating efficiency drop dramatically and the lifetime is short. Electronic-based methods also include frequency multipliers, gunn oscillators, bloch oscillators, quantum Cascade Lasers (QCLs), free Electron Lasers (FELs), and the like, which have the advantages of small size, compact structure, and the like, but due to the limitations of the processes and some core devices, only terahertz waves with a frequency of less than 1THz are often obtained. Terahertz coherent radiation sources based on semiconductor technology are developed rapidly and are considered to have a promising future, but at present, the terahertz coherent radiation sources are low in conversion efficiency and output power and can only operate under the conditions of ultralow temperature, large current and strong magnetic field. In addition, the quantum cascade laser known as the revolution of the middle and far infrared band laser technology only outputs terahertz waves with milliwatt power even if the temperature is used for developing the liquid nitrogen temperature through the energy band design, and is also restricted by the problems of complex growth technology, large working threshold current density, lower radiation frequency, serious optical loss and the like.
In the aspect of photonics, a photonics method is used for converting photon waves into terahertz waves in a down-conversion mode, the terahertz waves generated by the method have good directivity and coherence, and the frequency range can cover the whole terahertz wave band. The earliest researchers used high pressure mercury lamps with output powers up to 70 μ W in the range of 0-2 THz. Currently, optical methods mainly include terahertz wave gas lasers, ultrashort laser pulses, optical rectification capable of generating broadband subpicosecond terahertz radiation, photoconduction, plasma four-wave mixing, and the like, and nonlinear optical difference frequencies. However, most of the devices have the application problems of low energy conversion efficiency, large energy loss, large system-level elements, complexity, high price and the like.
Disclosure of Invention
Based on the above knowledge, it is found that there are inherent short ribs in terahertz wave sources obtained by either an electronic method or an optical method. The invention provides a brand-new terahertz wave source for the first time aiming at the problems of the existing terahertz wave source, directly uses graphene or a graphene composite material as a material and a main component of the terahertz wave source with the output frequency range of 0.1-10 THz, and solves the technical problems and application bottlenecks of the terahertz wave source in the prior art, such as complex component parts, high manufacturing cost, high preparation precision, low conversion efficiency, poor adjustability and the like.
The invention provides a terahertz wave radiation source based on a graphene material, which consists of radiation elements taking graphene or/and graphene composite materials as main bodies, can radiate terahertz waves with the frequency of 0.1-10 THz under the condition of electrification, and comprises the following components: the basic semiconductor layer is prepared from graphene or/and a graphene composite material and used for electrically exciting emission waves with the wavelength of mum-mm and providing a terahertz wave base source, wherein the basic semiconductor layer is formed on a base material, and the base material is provided with a surface; the metal compound, the adhesive resin, the conductive agent and the dispersion coupling agent form a transition transmission interaction layer of electromagnetic waves, the metal compound provides collision, enhancement and interference interaction for the electromagnetic waves to form terahertz waves, the adhesive resin is used for transmission interference of the electromagnetic waves and is used as a support body, the conductive agent is used for conductivity, and the dispersion coupling agent provides auxiliary dispersion stability; the graphene magnetic field emission layer is composed of graphene or/and a graphene composite material, is used for electrically exciting graphene surface plasmas, forms a graphene magnetic field with frequency modulation and emission functions, and has the same effect as a basic semiconductor layer and provides the same or different terahertz wave base source electromagnetic waves.
The graphene material comprises single layers, multiple layers, composite layers and blends, and the graphene composite material comprises physically and chemically modified graphene, graphite, carbon black, carbon nanotubes, carbon fibers, other carbon allotropes and one or more of the graphene-blended composite materials. The preparation method of the graphene comprises a single-layer or multi-layer graphene material prepared by an oxidation-reduction method, a Hummer method, a modified Hummer method, a mechanical stripping method, an electrical stripping method, epitaxial growth and a vapor deposition method, and the graphene material obtained by the derivation method. The physical modification method of graphene comprises mechanical ball milling, sanding and plasma treatment; chemical modifications include, but are not limited to, element doping, surface active group introduction, surface modification, amine functionalization, and combinations of such physical and chemical methods of preparation.
The metal compound in the transition transmission interaction layer refers to one or more compounds of oxides, chlorides, sulfides and carbonates of metal elements, the metal elements comprise one or more compounds of transition metals, metalloids, alkali metals and alkaline earth metals, the optimized metal compound is metal oxide TiO2, the bonding resin comprises one or more thermosetting and thermoplastic resins of phenolic resin, epoxy resin, amino resin, polyurethane, acrylic resin, polyesters and organic silicon, the optimized metal compound is epoxy resin, and the material proportion and basic parameters of the transmission interaction layer are as follows: 10-40 wt% of transition metal compound powder; 1-30 wt% of adhesive resin; 0.5 to 5 weight percent of dispersing coupling agent; 0.5 to 25 weight percent of conductive agent; the thickness of the transmission layer is more than or equal to 0.5 μm. The graphene magnetic field emission layer is constructed by compounding one or more of planar plate-shaped, curved plate-shaped, concave, conical, cylindrical, pin-shaped, rod-shaped or polygonal structures.
The graphene or/and graphene composite material is transferred and loaded on a substrate in a screen printing, extrusion coating, roller coating, wire bar coating, intaglio printing, letterpress printing, electrodeposition, electrophoresis or spraying mode, and the substrate is a rigid substrate or a flexible substrate.
On the whole, a terahertz wave radiation source based on graphene materials comprises a basic semiconductor layer (set A), a transition transmission interaction layer (set B) and a graphene magnetic field emission layer (set C) assembly, the arrangement mode can be one of ABC, AB and AC or any collocation and repeated arrangement between ABC, AB and AC to form an emission source, the included angle range of the arrangement angles of the components is 0-180 degrees, the components can be arranged side by side, in series and stacked according to needs to obtain terahertz waves with required dimensionality and volume meeting the specific power and specific frequency range, and the overall dimension of the radiation source can be expanded to 20 micrometers to the maximum extent. The maximum dominant temperature of the working condition can be 12V at room temperature, the operating temperature range is 10K-1573K, the working voltage range is 1-10000V, and the average power per square centimeter is output from several mu W-several million mW.
The outstanding technical effects of the invention compared with the prior art are explained in detail as follows:
(1) The invention provides a brand-new terahertz wave source for the first time, and a main body component is a transition transmission interaction layer consisting of a structural unit formed by graphene and graphene composite materials and a transition metal compound. The emission source has the advantages of simple manufacture, simple and convenient composition, short growth period, small processing requirement precision and the like, and can be completely applied to the existing market service society in a large scale.
(2) The radiation source provided by the invention completely comprises the whole terahertz wave frequency range, covers the whole 0.1-10 THz area, and is the terahertz wave in the real sense, and the terahertz wave with the frequency below 1THz can be obtained by a common electronic method. To a certain extent, the terahertz wave source composed of the graphene and the graphene composite material thereof provided by the invention does not belong to the scope of electron optical methods, does not belong to an optical emission source method, and is an emission mechanism directly acting on wave bands in an infrared region and a microwave region, so that higher conversion efficiency can be ensured. The conversion efficiency of the method can reach 10 < -4 > to 10 < -2 >, and is improved by 1 to 2 orders of magnitude compared with the conversion efficiency of an optical method.
(3) The radiation source provided by the invention can be expanded to direct current and alternating current, has low working voltage, and can generate terahertz waves with the power of more than mW even if the direct current is less than 24V, which is a level which cannot be reached by the terahertz wave radiation element in the prior art, and compared with the existing terahertz wave source, the terahertz wave radiation element does not need to work under ultrahigh voltage and current. In addition, compared with a quantum cascade laser terahertz wave source which needs liquid nitrogen cooling work, the terahertz wave source can be stably produced without a specific cooling system at room temperature, so that the terahertz wave source can be expected to be applied to the application fields of safety guarantee, biology, environment, communication and the like which utilize terahertz waves for a long time in a large scale and all time, and make greater contribution to development and progress of the terahertz wave source.
(4) The terahertz wave source constructed by the invention has the advantages of simple structure, single component, high flexibility and adjustability, and can be suitable for the strict requirements of ultra-thin, compactness, arbitrary radian, dimensionality and the like. The overall structure scale can reach the millimeter scale, and the average transmitted terahertz wave power can reach the mW level, which is a level that cannot be reached by other terahertz wave sources. In addition, because an additional light source and a specific light path are not required, the size can be expanded to any size by microscopic adjustment to be suitable for a special field.
(5) The preferred terahertz wave source can provide an ultrathin and ultralight terahertz wave emission source, and is particularly suitable for being used in special fields such as portable fields, outdoor fields and handheld fields. Because the provided terahertz wave source body is prepared from low-density inorganic nonmetallic materials, a small amount of transition metal compounds and organic polymers, the portability of the terahertz wave source body is maintained even under large size and large dimension.
(6) The terahertz wave source constructed by the invention can realize ordered adjustment in the frequency range of 0.1-10 THz, and has convenient adjustment and adjustable wavelength range. The method mainly utilizes the excellent photoelectric characteristics of graphene and graphene composite materials thereof, and more importantly, utilizes the fact that graphene is a high-efficiency high-flux frequency modulator (realized by adjusting the Fermi level of graphene) at room temperature. In addition, the invention also provides a method for adjusting terahertz waves by adjusting the applied voltage of the layer, the three-dimensional direction between the semiconductor base layer and the graphene magnetic field and the type of the transmission interaction layer.
Drawings
Fig. 1 is a schematic structural diagram of embodiment 1, in which a terahertz wave source is an element having a three-layer macrostructure, a layer a is a semiconductor base layer, a layer B is a transmission interaction layer containing a transition metal chemical, and a layer C is a graphene magnetic field emission layer.
FIG. 2 is a graph showing the change of the mean power of the terahertz wave with time parameters in the range of 0.1 to 10THz of the frequency emitted from the terahertz wave radiation source prepared in example 1, wherein the working voltage of the radiation source is 24V direct current, the area is 400X 400mm, and the overall thickness is 2mm. The terahertz wave source is composed of three layers of elements with macroscopic structures, wherein the layer A is a semiconductor base layer with the thickness of 0.8mm, the layer B is a TiO2 transmission interaction layer with the thickness of 0.4mm, and the layer C is a graphene magnetic field emission layer with a concave structure with the thickness of 0.8 mm. Under the test conditions, a silicon chip window with the diameter of 22mm is added in front of a terahertz wave source, the distance between the terahertz wave source and a terahertz wave detector is 120mm, and the frequency of a wave folder is 61.6Hz.
Detailed Description
The present invention will be described in further detail with reference to specific examples and drawings, but the present invention is not limited to the examples.
Example 1
Firstly, a graphene semiconductor base layer is constructed in a chemical vapor deposition mode, then the Fermi level of graphene is adjusted through chemical nitrogen doping to realize the characteristics of a graphene semiconductor, and then the graphene semiconductor base layer is transferred to a polyester PET film to form a conductive network layer with a certain structure. The graphene mainly comprises single-layer graphene and a small amount of multi-layer graphene, and forms a semiconductor base layer A.
The material of the transmission interaction layer is preferably TiO metal compound 2 The nano oxide layer and the bonding resin are high-density polyethylene materials. The material ratio and basic parameters of the transmission interactive layer are as follows: 15 wt% of transition metal compound powder, 45 wt% of bonding resin, 2 wt% of dispersion coupling agent, 38 wt% of conductive agent, and the thickness of a transmission layer is 0.4mm, and the layer is marked as a layer B.
Graphene with the single layer rate of 80% is subjected to surface organic silicon modification treatment, and then is coated in a concave template by an electrophoresis graphene paint method to construct a multi-dimensional graphene magnetic field C layer.
And (3) adjusting the A layer and the C layer of the prepared ABC layer to 10 degrees in a macroscopic view to obtain a main emission window, then switching 24V direct current between the A layer and the C layer, and obtaining the average power of the THz terahertz wave with the frequency of 0.1-10 mW at the working temperature of 100 ℃. Test report certificate number: GFJGJL1008180234006, national defense science and technology industry optics first-order metering station (optical calibration testing laboratory at the institute of optics, west ann). The test condition is that a silicon chip window with the diameter of 22mm is added in front of the terahertz wave source; the distance between the terahertz wave source and the terahertz wave emitter is 120mm; chopper frequency 61.6Hz; terahertz wave radiation power meter, certificate number: GXjg2017-1690. Technical documentation for calibration: JJF (military) 118-2016 terahertz wave radiation parameter calibration standard
Example 2
The method comprises the steps of constructing a graphene semiconductor base layer by adopting an electrodeposition method, adding melamine to carry out nitrogen doping in the electrodeposition process, directly transferring the nitrogen doped graphene semiconductor base layer into an epoxy resin plate, and processing the nitrogen doped graphene semiconductor base layer to form a conductive network layer of a structure. The single-layer rate of the active graphene in the electrodeposition liquid reaches 90%, and the other layers are multi-layer graphene to form a semiconductor base layer A.
The material of the transmission interaction layer is preferably TiO metal compound 2 The nano oxide layer and the bonding resin are high-density polyethylene materials. The material ratio and basic parameters of the transmission interactive layer are as follows: 20 wt% of transition metal compound powder, 40wt% of bonding resin, 2 wt% of dispersion coupling agent, 0.5 wt% of conductive agent, and the thickness of a transmission layer is 0.4mm, and the layer is marked as a layer B.
Graphene magnetic field emission layers in the terahertz wave source are formed by performing surface organic silicon modification treatment on graphene with a single layer rate of 80% and then coating the graphene into a concave template by an electrophoresis graphene paint method to construct a multi-dimensional graphene magnetic field C layer.
And (3) obtaining a main emission window of the prepared ABC layer, wherein the layer A and the layer C are adjusted to be 15 degrees in a macroscopic view, then accessing 220V alternating current to each layer, and obtaining the terahertz wave with the frequency of 0.1-10 THz with the average power of 3.360 mW at room temperature.
Example 3
The graphene slurry is printed into a ceramic substrate by adopting a screen printing mode, metal nano elements are introduced to modify graphene by an electroplating mode, and then a conductive network layer of the structure is formed by processing. The single-layer rate of the graphene slurry reaches 99%, and the other graphene layers are multilayer graphene to form a semiconductor base layer A.
The material of the transmission interaction layer is preferably CaCO as the metal compound 3 The nano oxide layer and the bonding resin are low-temperature resistant materials. The material ratio and basic parameters of the transmission interactive layer are as follows: 20 wt% of transition metal compound powder, 40wt% of bonding resin, 2 wt% of dispersion coupling agent, 0.5 wt% of conductive agent, and the thickness of a transmission layer is 0.4mm, and the layer is marked as a layer B.
Graphene magnetic field emission layers in the terahertz wave source are formed by performing surface organic silicon modification treatment on graphene with a single layer rate of 80% and then directly spraying the graphene magnetic field emission layers to polyester materials in a spraying mode to construct a multi-dimensional graphene magnetic field C layer.
And (3) obtaining a main emission window on the prepared ABC layer, wherein the layer A and the layer C are adjusted to be 15 degrees in a macroscopic view, then accessing 220V alternating current to each layer, and obtaining the terahertz wave with the frequency of 0.1-10 THz with the average power of 1.059mW at the working temperature of-30 ℃.
Claims (9)
1. A terahertz wave radiation source based on graphene materials is characterized by comprising radiation elements taking graphene or/and graphene composite materials as main bodies, and capable of radiating terahertz waves with the frequency of 0.1-10 THz under the electrified condition, and comprises: the base semiconductor layer is prepared from graphene or/and a graphene composite material and is used for electrically exciting emission waves with the wavelength of mum-mm and providing a terahertz wave base source, wherein the base semiconductor layer is formed on a base material, and the base material is provided with a surface; the metal compound, the adhesive resin, the conductive agent and the dispersion coupling agent form a transition transmission interaction layer of electromagnetic waves, the metal compound provides collision, enhancement and interference interaction for the electromagnetic waves to form terahertz waves, the adhesive resin is used for transmission interference of the electromagnetic waves and is used as a support body, the conductive agent is used for conductivity, and the dispersion coupling agent provides auxiliary dispersion stability; the graphene magnetic field emission layer is composed of graphene or/and a graphene composite material, is used for electrically exciting graphene surface plasmas, forms a graphene magnetic field with frequency modulation and emission functions, and has the same effect as a basic semiconductor layer and provides the same or different terahertz wave base source electromagnetic waves.
2. The terahertz wave radiation source based on the graphene material, as claimed in claim 1, wherein the graphene material includes a single layer, multiple layers, composite layers and blends, and the graphene composite material includes one or more of physically and chemically modified graphene, graphite, carbon black, carbon nanotubes and carbon fibers blended with graphene.
3. The terahertz wave radiation source based on the graphene material is characterized in that the graphene is prepared by a single-layer or multi-layer graphene material prepared by a redox method, a Hummer method, a modified Hummer method, a mechanical stripping method, an electrical stripping method, an epitaxial growth method and a vapor deposition method.
4. The terahertz wave radiation source based on the graphene material as claimed in claim 2, wherein the physical graphene modification method includes but is not limited to mechanical ball milling, sand milling, plasma treatment, the chemical modification includes but is not limited to element doping, surface active group introduction, surface modification, amine functionalization, and the combined preparation of physical and chemical methods.
5. The terahertz wave radiation source based on graphene materials of claim 1, wherein the metal compound refers to one or more of oxides, chlorides, sulfides and carbonates of metal elements, the metal elements include one or more of transition metals, metalloids, alkali metals and alkaline earth metals, the binding resin includes but is not limited to thermosetting and thermoplastic resins of one or more of phenolic resin, epoxy resin, amino resin, polyurethane, acrylic resin, polyesters and silicone, and the material composition and basic parameters of the transmission interaction layer are as follows: 10-40 wt% of transition metal compound powder; 1-30 wt% of adhesive resin; 0.5 to 5 weight percent of dispersing coupling agent; 0.5 to 25 weight percent of conductive agent; the thickness of the transmission layer is more than or equal to 0.5 μm.
6. The terahertz wave radiation source based on graphene materials as claimed in claim 1, wherein the structure of the graphene magnetic field emission layer comprises a planar plate, a curved plate, a concave, a convex, a conical, a cylindrical, a tubular, a rod or a polygonal structure.
7. The terahertz wave radiation source based on the graphene material as claimed in any one of claims 1 to 5, wherein the graphene or/and graphene composite material is transfer-loaded on a substrate in a screen printing, extrusion coating, roll coating, wire bar coating, gravure printing, letterpress printing, electrodeposition, electrophoresis or spraying manner, and the substrate is a rigid substrate or a flexible substrate.
8. The terahertz wave radiation source based on the graphene material as claimed in claim 1, wherein a basic semiconductor layer is set as A, a transition transmission interaction layer is set as B, a graphene magnetic field emission layer is set as C, the basic semiconductor layer, the transition transmission interaction layer and the graphene magnetic field emission layer are arranged in any collocation and repeated arrangement of one or more of ABC, AB and AC, the included angle range of the arrangement angle of the components is 0-180 degrees, the components are arranged side by side, in series and stacked as required, terahertz waves with required dimension and volume meeting specific power and specific frequency range are obtained, and the minimum dimension of the whole radiation source is extended to 20 μm and is not limited at most.
9. The terahertz wave radiation source based on graphene material according to claim 1, which has a working temperature of 10K to 1573K, a working voltage range of 1 to 10000V, and an output of several μ W to several million mW per square centimeter of average power.
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| CN106200016A (en) * | 2016-07-25 | 2016-12-07 | 上海师范大学 | A kind of Terahertz Graphene microstructure Modulation device |
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