CN110512282B - Implementation method of novel terahertz radiation source - Google Patents
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- CN110512282B CN110512282B CN201910939038.8A CN201910939038A CN110512282B CN 110512282 B CN110512282 B CN 110512282B CN 201910939038 A CN201910939038 A CN 201910939038A CN 110512282 B CN110512282 B CN 110512282B
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- 239000000758 substrate Substances 0.000 claims abstract description 34
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- 229910020054 Mg3Bi2 Inorganic materials 0.000 claims abstract description 17
- 239000011669 selenium Substances 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 230000008020 evaporation Effects 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 230000003287 optical effect Effects 0.000 claims abstract description 7
- 238000007872 degassing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 5
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000012512 characterization method Methods 0.000 claims abstract description 3
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 3
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- 238000005498 polishing Methods 0.000 claims abstract 2
- 239000011241 protective layer Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052594 sapphire Inorganic materials 0.000 claims description 5
- 239000010980 sapphire Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
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- 238000000151 deposition Methods 0.000 abstract description 2
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910007709 ZnTe Inorganic materials 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
Abstract
The invention discloses a method for realizing a novel terahertz radiation source, which comprises a material preparation method and a test method, and comprises the following steps: s1: firstly, conveying a substrate with double-sided or single-sided polishing into an ultrahigh vacuum MBE cavity; s2: then heating and degassing the substrate in an ultra-high vacuum MBE cavity; s3: adjusting the beam sizes of the two evaporation sources by controlling the temperature of a magnesium (Mg) source and a bismuth (Bi) source, and further adjusting the proportion of the Mg source and the Bi source evaporated on the substrate; s4: simultaneously depositing and combining a Mg source and a Bi source on a substrate to obtain single crystal Mg3Bi2A film; s5: after the temperature of the substrate is reduced to room temperature, the substrate is heated to Mg3Bi2Covering the single crystal thin film with an amorphous selenium (Se) film to prevent Mg3Bi2Oxidizing; s6: utilizing optical pumping terahertz detection system to detect Mg3Bi2And performing terahertz radiation characterization on the monocrystalline film. The method has the advantages of simple operation, high quality of the monocrystalline film and strong repeatability, and can provide effective technical guidance for the growth of the monocrystalline film material and the generation of the terahertz radiation source.
Description
Technical Field
The invention relates to the field of terahertz functional materials, in particular to a novel terahertz radiation source realization method.
Background
Terahertz (THz) waves are electromagnetic waves in the electromagnetic spectrum in the frequency band of 0.1THz-10THz, with corresponding wavelengths of 30-3000 μm, also known as submillimeter waves. The frequency band has many unique properties, such as lower photon energy (0.4-40meV), strong transmittance to nonpolar materials, the same wave band with the vibration and rotation energy of more macromolecular substances, strong absorption by water, and the like. Based on the properties, the terahertz wave has wide application prospects in a plurality of fields such as medical imaging, nondestructive testing, wave spectrum analysis, space communication, safety inspection and the like. The efficient terahertz radiation source is the key to the application of the terahertz technology. Many methods for generating terahertz radiation exist, a backward wave tube, a solid-state frequency doubling source and the like based on the electronic technology work below 1THz and extend towards the high-frequency direction, and the output power is usually in the magnitude of microwatts to milliwatts; the quantum cascade laser, the free electron laser and the like based on the photonics technology have the working frequency extending to the low-frequency direction and larger output power; and an ultrafast photoconductive device based on an ultrafast laser technology, etc., the operating frequency is near 1THz and develops to high frequency and low frequency simultaneously, and the device has the advantages of narrow pulse width, high peak power, etc., but has the problems of low energy conversion efficiency and average output power. Therefore, exploring a new radiation source that can simultaneously satisfy room temperature operation, high output power, continuous coordination and miniaturization becomes an important development target in the current terahertz field.
The method has the advantages that a novel terahertz radiation source is explored, the terahertz radiation intensity of the existing material is improved, the terahertz radiation characteristic of a new material needs to be continuously researched, and the new material is searched to serve as the terahertz radiation source; mg (magnesium)3Bi2The material is a novel topological pitch line semimetal (NLS) material, which is a novel topological solid phase, two energy bands are intersected to form a one-dimensional closed ring or linear degeneracy, and the two energy bands have the same sign in the radial inclination direction of the ring; this may result in different magnetic, optical and transmission characteristics compared to conventional nodal loops; due to time reversal symmetry, the surface state of the crystal has two closed electron scattering paths, one path generates Berry phase with the magnitude of pi when passing through a single Dirac cone and generates destructive quantum interference with the other path, so that Mg is improved3Bi2So that it has semi-metallic characteristics; previous pair of Mg3Bi2The research is mainly focused on the good thermoelectric performance of the material, no research report related to the material in terahertz waves is seen at present, and therefore, a novel topological pitch line semimetal Mg is provided3Bi2A method for applying a single crystal film to a terahertz radiation source is provided.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a novel implementation method of a terahertz radiation source.
The implementation method of the novel terahertz radiation source comprises a material preparation method and a test method, and comprises the following steps:
s1: firstly, conveying a double-sided or double-sided polished substrate into an ultrahigh vacuum MBE cavity;
s2: then heating and degassing the substrate in an ultra-high vacuum MBE cavity;
s3: adjusting the beam sizes of the two evaporation sources by controlling the temperature of a magnesium (Mg) source and a bismuth (Bi) source, and further adjusting the proportion of the Mg source and the Bi source evaporated on the substrate;
s4: simultaneously depositing and combining the Mg source and the Bi source on the substrate to obtain Mg3Bi2A single crystal thin film;
s5: after the temperature of the substrate is reduced to room temperature, the substrate is heated to Mg3Bi2The film is covered with an amorphous selenium (Se) film to prevent Mg3Bi2An oxidized protective layer;
s6: utilizing optical pumping terahertz detection system to detect Mg3Bi2And performing terahertz radiation characterization on the film.
Preferably, the substrate in S1 may be an insulator that is transparent to THz waves, such as sapphire, quartz, and glass.
Preferably, the heating in S2 is by indirect heating, and the degassing time is 2 h.
Preferably, the temperature of the evaporation source in S3 can vary within a certain range, such as Mg in the range of 300 to 600 ℃, Bi in the range of 400-700 ℃, and the beam ratio of the Mg source to the Bi source is greater than 3:2, the growth temperature of the substrate can be varied within the range of 250 ℃ to 450 ℃.
Preferably, the protective layer covered in S5 may be Bi, Te, Al2O3, SiO2, or the like which is transparent to THz waves and has an air-barrier effect.
Preferably, Mg in S63Bi2The film has the characteristic of optical pumping radiation terahertz waves, and can be made into THz radiation sources and other related devices.
Preferably, the above Mg is added3Bi2The monocrystalline film is applied to terahertz detection.
The invention has the beneficial effects that: during growth, the evaporation sources of Mg and Bi are heated according to a specific beam current ratio, so that atoms or molecules of Mg and Bi are simultaneously deposited on a sapphire substrate at a specific temperature, and a Se protective layer is covered; the topological nodal line semimetal has a novel topological surface state, due to time reversal symmetry, two closed electron scattering paths on the surface state, one closed electron scattering path generates a Berry phase with the size pi when passing through a single Dirac cone, and destructive quantum interference is generated with the other closed electron scattering path, so that Mg is improved3Bi2Is provided with Mg3Bi2The semi-metallic nature of (a); therefore, when the terahertz radiation source is optically pumped, a larger transient photocurrent can be generated in a short time, so that a stronger terahertz radiation signal can be measured at room temperature.
Drawings
FIG. 1 is a reflection type high energy electron diffraction pattern of a sapphire substrate after high temperature degassing in an embodiment of the present invention.
FIG. 2 shows high quality Mg produced in examples of the present invention3Bi2Reflective high energy electron diffraction patterns of thin films.
FIG. 3 is Mg after Se film covering in an embodiment of the present invention3Bi2Reflective high energy electron diffraction patterns of thin films.
FIG. 4 is Mg after Se film covering in an embodiment of the present invention3Bi2X-ray diffraction pattern of the film.
FIG. 5 is Mg covering Se layer in an embodiment of the invention3Bi2The film optically pumps terahertz radiation signals under different power densities.
FIG. 6 shows an embodiment of the present invention5 Mg overlying Se layer3Bi2Spectrograms of optically pumped terahertz radiation signals of the film at different power densities after Fourier transformation.
FIG. 7 is Mg covering Se layer in an embodiment of the invention3Bi2The linear relation between the highest signal intensity of the terahertz radiation of the film and the power density of the pump light.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Examples
The embodiment provides a method for realizing a novel terahertz radiation source, which comprises a material preparation method and a material testing method and comprises the following steps:
s1: firstly, Al with the crystal face direction of (0001), the size of 5mm 10mm 0.5mm and polished double sides or single sides is prepared2O3Transferring the substrate into an ultra-high vacuum MBE cavity, wherein the vacuum is required to be better than 2.0 multiplied by 10 < -10 > mBar;
s2: al is heated indirectly in MBE cavity2O3The substrate is at about 700 ℃ until the system is recovered to the back substrate vacuum, so as to thoroughly remove the water vapor and organic matters adsorbed on the surface;
s3: setting the temperature of a Mg evaporation source to be 400 ℃, setting the temperature of a Bi source to be 580 ℃, and controlling the beam current ratio of the Mg source to the Bi source to be slightly more than 3: 2. the substrate is heated indirectly to stabilize the temperature of the substrate at about 350 ℃. The time required for heating the evaporation source and the substrate to be stable is about 20-30 minutes;
s4: opening the baffle switches of the Mg evaporation source and the Bi evaporation source, starting timing while opening the substrate baffle, and controlling the growth time of the sample to be 30 min. After the growth is finished, closing the Mg and Bi evaporation sources and the substrate baffle plate, and cooling the temperature to room temperature;
s5: the Se evaporation source temperature is set to 170 ℃, the temperature of the evaporation source is increased to the specified temperature, and the temperature of the substrate is reduced to room temperature, and Mg is added3Bi2An amorphous Se film is deposited on the film for 5 min to prevent oxygen and moisture and Mg in the air3Bi2Film connectorContacting;
s6: pairing Mg with optically pumped terahertz detection (OPTP) system3Bi2The film is characterized by terahertz radiation. With the regenerative amplifier system, a 1KHz repetitive optical laser pulse is provided with a center wavelength of 800nm and a pulse width of 100fs (full width at half maximum). The energy of a single pulse of the OPTP device was constant at 6 mJ. In the presence of Mg3Bi2In the excitation of the film terahertz radiation, the optical pumping adopts split 800nm laser beams, the diameter of a light spot is 5mm, and the Mg is ensured3Bi2The film is uniformly excited by light. The detection of THz is based on a 1mm thick nonlinear crystal (ZnTe). Within a certain time window, the time domain waveform of THz is recorded by detecting the movement of light through the delay line.
The degassing time in S2 was 2 h.
In this embodiment, Mg may be added3Bi2The single crystal film is applied to terahertz radiation source devices and other related devices.
During growth, the evaporation sources of Mg and Bi are heated according to a specific beam current ratio, so that atoms or molecules of Mg and Bi are simultaneously deposited on a sapphire substrate at a specific temperature, and a Se protective layer is covered; the topological nodal line semimetal has a novel topological surface state, due to time reversal symmetry, two closed electron scattering paths on the surface state, one closed electron scattering path generates a Berry phase with the size pi when passing through a single Dirac cone, and destructive quantum interference is generated with the other closed electron scattering path, so that Mg is improved3Bi2Is provided with Mg3Bi2The semi-metallic nature of (a); therefore, when the terahertz radiation detector is optically pumped, a large transient photocurrent can be generated in a short time, so that a strong terahertz radiation signal can be detected at room temperature.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, but to assist understanding of the method of the present invention and the core concept thereof. It will be apparent to those skilled in the art that various changes and modifications can be made in the form and details of the above-described embodiments without departing from the principles of the invention. All obvious changes and modifications which are obvious and encompassed by the technical solution of the present invention are within the scope of the present invention.
Claims (6)
1. The implementation method of the terahertz radiation source comprises a material preparation and test method and is characterized by comprising the following steps:
s1: firstly, conveying a substrate with double-sided or single-sided polishing into an ultrahigh vacuum MBE cavity;
s2: then heating and degassing the substrate in an ultra-high vacuum MBE cavity;
s3: adjusting the beam sizes of the two evaporation sources by controlling the temperature of a magnesium (Mg) source and a bismuth (Bi) source, and further adjusting the proportion of the Mg source and the Bi source evaporated on the substrate;
s4: mg source and Bi source are simultaneously deposited on the substrate and combined to obtain single-crystal Mg3Bi2A film;
s5: after the temperature of the substrate is reduced to room temperature, the substrate is heated to Mg3Bi2The film is covered with an amorphous selenium (Se) film to prevent Mg3Bi2An oxidized protective layer;
s6: utilizing optical pumping terahertz detection system to detect Mg3Bi2And performing terahertz radiation characterization on the monocrystalline film.
2. The method for implementing the terahertz radiation source according to claim 1, wherein the substrate in S1 is sapphire or quartz.
3. The method for implementing the terahertz radiation source as claimed in claim 1, wherein the temperature of the evaporation source in S3 can be varied within a certain range, Mg is within a range of 300 to 600 ℃, Bi is within a range of 400-700 ℃, the beam ratio of the Mg source and the Bi source is greater than 3:2, and the growth temperature of the substrate can be varied within a range of 250-450 ℃.
4. The method for implementing the terahertz radiation source of claim 1, wherein the protective layer covered in S5 is Al2O3Or SiO2。
5. The method of claim 1, wherein the S6 contains Mg3Bi2The single crystal thin film is a topological nodal line type semimetal.
6. The method of claim 1, wherein the Mg is added to the solution3Bi2The monocrystalline film is applied to terahertz detection.
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| CN103308181A (en) * | 2013-04-27 | 2013-09-18 | 北京理工大学 | VOx terahertz uncooled focal plane detector component |
| CN103499534A (en) * | 2013-07-25 | 2014-01-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-sensitivity terahertz microfluidic channel sensor and preparation method thereof |
| CN103575407A (en) * | 2012-07-18 | 2014-02-12 | 北京大学 | Terahertz radiation detector |
| CN103606585A (en) * | 2013-11-25 | 2014-02-26 | 电子科技大学 | Terahertz room temperature detector with high-absorbability structure and manufacturing method thereof |
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| CN107425081B (en) * | 2017-06-28 | 2019-02-26 | 中国人民解放军国防科学技术大学 | Topological insulator array type optical electric explorer and its preparation method and application based on graphene class two-dimensional material protection layer |
| CN109913945B (en) * | 2019-03-14 | 2021-04-02 | 电子科技大学 | Method for growing bismuth selenide high-index surface single crystal film on silicon (211) substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103575407A (en) * | 2012-07-18 | 2014-02-12 | 北京大学 | Terahertz radiation detector |
| CN103308181A (en) * | 2013-04-27 | 2013-09-18 | 北京理工大学 | VOx terahertz uncooled focal plane detector component |
| CN103499534A (en) * | 2013-07-25 | 2014-01-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | High-sensitivity terahertz microfluidic channel sensor and preparation method thereof |
| CN103606585A (en) * | 2013-11-25 | 2014-02-26 | 电子科技大学 | Terahertz room temperature detector with high-absorbability structure and manufacturing method thereof |
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