CN109411563B - Substrate precursor for terahertz wave detector and preparation method thereof - Google Patents
Substrate precursor for terahertz wave detector and preparation method thereof Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 43
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- 238000002955 isolation Methods 0.000 claims description 28
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000012141 concentrate Substances 0.000 claims description 24
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 24
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 12
- 229910052772 Samarium Inorganic materials 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 12
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims description 12
- HGQSXVKHVMGQRG-UHFFFAOYSA-N dioctyltin Chemical compound CCCCCCCC[Sn]CCCCCCCC HGQSXVKHVMGQRG-UHFFFAOYSA-N 0.000 claims description 12
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- 229940071125 manganese acetate Drugs 0.000 claims description 12
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 12
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 12
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 12
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 12
- 239000002041 carbon nanotube Substances 0.000 claims description 9
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 9
- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- LTSCBXDGJFSJMR-UHFFFAOYSA-N 4-methylcyclohexa-2,4-diene-1,1-diamine Chemical compound CC1=CCC(N)(N)C=C1 LTSCBXDGJFSJMR-UHFFFAOYSA-N 0.000 claims description 8
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- ODVRHJKVXOGKEJ-UHFFFAOYSA-N iron 5,10,15,20-tetraphenyl-21,23-dihydroporphyrin Chemical compound [Fe].c1cc2nc1c(-c1ccccc1)c1ccc([nH]1)c(-c1ccccc1)c1ccc(n1)c(-c1ccccc1)c1ccc([nH]1)c2-c1ccccc1 ODVRHJKVXOGKEJ-UHFFFAOYSA-N 0.000 claims description 8
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- ZWYCMWUUWAFXIA-UHFFFAOYSA-N iron(2+);5,10,15,20-tetraphenylporphyrin-22,23-diide Chemical compound [Fe+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C2=CC=C([N-]2)C(C=2C=CC=CC=2)=C2C=CC3=N2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 ZWYCMWUUWAFXIA-UHFFFAOYSA-N 0.000 claims description 5
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- 238000001514 detection method Methods 0.000 abstract description 39
- 229910002601 GaN Inorganic materials 0.000 abstract description 25
- RNQKDQAVIXDKAG-UHFFFAOYSA-N aluminum gallium Chemical compound [Al].[Ga] RNQKDQAVIXDKAG-UHFFFAOYSA-N 0.000 abstract description 12
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 abstract description 9
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- 229910002704 AlGaN Inorganic materials 0.000 description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 6
- 229910052733 gallium Inorganic materials 0.000 description 6
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000001328 terahertz time-domain spectroscopy Methods 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/184—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP
- H01L31/1844—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP comprising ternary or quaternary compounds, e.g. Ga Al As, In Ga As P
- H01L31/1848—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP comprising ternary or quaternary compounds, e.g. Ga Al As, In Ga As P comprising nitride compounds, e.g. InGaN, InGaAlN
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/112—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor
- H01L31/113—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor
- H01L31/1136—Devices sensitive to infrared, visible or ultraviolet radiation characterised by field-effect operation, e.g. junction field-effect phototransistor being of the conductor-insulator-semiconductor type, e.g. metal-insulator-semiconductor field-effect transistor the device being a metal-insulator-semiconductor field-effect transistor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the technical field of detectors, and particularly relates to a substrate precursor for a terahertz wave detector and a preparation method thereof. An aluminum gallium nitride/gallium nitride high electron mobility field effect transistor (HEMT) is used as a basic structure, and an aluminum gallium nitride/gallium nitride layer is prepared by a substrate design and an epitaxial method; and then preparing an active region table board, a gate medium, an ohmic contact window and an electrode, wherein the obtained two-dimensional electron gas in the field effect transistor has higher electron concentration and mobility, so that the spectrum detection device for realizing high-speed, high-sensitivity and high-signal-to-noise ratio detection on the THz wave at room temperature is obtained, and the detection on the terahertz wave is finally realized.
Description
The invention belongs to divisional application of invention application with the name of a terahertz wave detector and a preparation method thereof, application number of 201710495198.9 and application date of 2017, 6 months and 26 days, and belongs to a product and a preparation method thereof.
Technical Field
The invention belongs to the technical field of detectors, and particularly relates to a substrate precursor for a terahertz wave detector and a preparation method thereof.
Background
Terahertz (THz) radiation is a general term for electromagnetic radiation of a specific wavelength band, and generally refers to electromagnetic waves with a frequency in the range of 0.1THz to 10THz (with a wavelength of 3mm to 30 um), which are located between microwave and infrared radiation in the electromagnetic spectrum. In the field of electronics, electromagnetic waves in this band are also called millimeter waves and submillimeter waves; and in the field of spectroscopy, it is also known as far infrared.
Terahertz radiation is of great interest because of its many unique properties and broad application prospects. The terahertz wave radiation source includes: wide frequency, perspective, safety and other characteristics, so it has important application prospect in the basic fields of physics, chemistry, biomedicine and the like, and in the aspects of nondestructive imaging, safety inspection, spectral analysis and radar communication.
Like a terahertz radiation source, terahertz detection is also another key technology in terahertz science and technology, and is also another key link for putting the terahertz technology into practical application. At present, the terahertz signal detection technology can be divided into a coherent pulse time domain continuous wave detection technology and an incoherent direct energy detection technology in principle. The terahertz pulse time-domain continuous wave detection technology based on the coherent technology adopts a mode similar to terahertz pulse generation to carry out coherent detection, and one detection method is called as a terahertz time-domain spectroscopy technology; the other type adopts a superheterodyne detector at the low-frequency end of the terahertz wave. The main detection methods include thermal radiation detection, Fourier transform spectroscopy, time domain spectroscopy, heterodyne detection and terahertz quantum well infrared photon detection. In the development and utilization of terahertz wave bands, the detection of terahertz signals has great significance. On one hand, due to the fact that the output power of the terahertz radiation source is low, the background noise of the terahertz radiation in a frequency range is large, water vapor attenuation is serious and the like, terahertz radiation signals reflected from a target are lower, and compared with optical waveband electromagnetic waves with shorter wavelengths, the energy of terahertz wave photons is low, and the background noise generally occupies a significant position. On the other hand, with the deep development of the terahertz technology in various fields, particularly in the military field, the continuous improvement of the detection sensitivity becomes a necessary requirement.
Because the radiation power of the existing terahertz light source is generally low, and the existing terahertz wave detector generally has the defects of low response speed (pyroelectric detector), narrow detection frequency (schottky diode), poor sensitivity (Golay cell detector) and low-temperature operation (bolometer), the development of the terahertz wave detector which is high in speed, high in sensitivity and signal to noise and can operate at room temperature is particularly important.
In the former detector, a three-pole coupling antenna is integrated with an HEMT device as a source, a drain and a gate electrode at the same time, the gate electrode antenna and the source electrode antenna are in the same plane, and the metal gate electrode plays a large role in shielding a transverse electric field at a 2 DEG position under the gate, so that the coupling efficiency of the antenna is low and the responsivity of the device is low.
Therefore, researchers have long been eager to develop a mature commercial terahertz detector with high sensitivity, wide detection frequency, small volume, high speed, low price and room temperature operation so as to greatly promote the development and application of the THz technology.
Disclosure of Invention
The invention discloses a terahertz wave detector and a preparation method thereof, wherein an aluminum gallium nitrogen/gallium nitrogen high electron mobility field effect transistor (HEMT) is used as a basic structure, two-dimensional electron gas in the HEMT has higher electron concentration and mobility, a spectrum detection device for realizing high-speed, high-sensitivity and high signal-to-noise ratio detection on THz waves under the room temperature condition is obtained, and the detection on the terahertz waves is finally realized.
The invention adopts the following technical scheme:
a preparation method of a terahertz wave detector comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) sequentially coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on a heat-resistant substrate to obtain a substrate; drying at room temperature after each coating;
(6) preparing an aluminum gallium nitride/gallium nitride layer on a substrate by an epitaxial method; and then preparing an active region table board, a gate medium, an ohmic contact window and an electrode so as to obtain the terahertz wave detector.
The invention also discloses a preparation method of the terahertz wave detection device, which comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) sequentially coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on a heat-resistant substrate to obtain a substrate; drying at room temperature after each coating;
(6) preparing an aluminum gallium nitride/gallium nitride layer on a substrate by an epitaxial method; then preparing an active region table board, a gate medium, an ohmic contact window and an electrode so as to obtain a terahertz wave detector; and packaging the terahertz wave detector to obtain the terahertz wave detection device.
The invention also discloses a preparation method of the terahertz wave detection system, which comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) sequentially coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on a heat-resistant substrate to obtain a substrate; drying at room temperature after each coating;
(6) preparing an aluminum gallium nitride/gallium nitride layer on a substrate by an epitaxial method; then preparing an active region table board, a gate medium, an ohmic contact window and an electrode so as to obtain a terahertz wave detector; packaging the terahertz wave detector to obtain a terahertz wave detection device; and combining the terahertz wave detection device with a support, a computer and an indicator lamp to obtain the terahertz wave detection system.
In the invention, creativity lies in the preparation of the substrate, the substrate in the prior art is completely overturned, and the subsequent further operation is carried out on the substrate, for example, an aluminum gallium nitride/gallium nitride layer is prepared on the substrate by an epitaxial method; then, preparing an active region table top, a gate medium, an ohmic contact window and an electrode, which belong to the prior art, and designing according to required parameters can not influence the technical effect of the invention; packaging the terahertz wave detector to obtain the terahertz wave detection device, wherein the operation of the terahertz wave detection device can also be carried out according to chip epoxy packaging; the terahertz wave detection device is combined with the support, the computer and the indicator light to obtain the terahertz wave detection system which can be operated according to mechanical design and computer connection. The terahertz wave detection system can be used for accurately and stably detecting the terahertz waves in the environment.
In the invention, the mass ratio of ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol, propionic acid, potassium hydroxide methanol solution, tert-butyl peroxybenzoate, manganese acetate, cobalt nitrate, water and samarium trimaran is 15: 45: 38: 150: 80: 50: 3: 20: 30: 100: 2; the mass ratio of the centrifugal precipitate, polyvinyl alcohol, hydrogen peroxide, iron tetraphenylporphyrin, 4-diaminophenylmethane and ethyl orthosilicate is 15: 55: 5: 0.1: 40: 50; the mass ratio of the graphene oxide to the epoxy resin to the acetone to the glyceryl monostearate to the diphenyl silanediol to the paraffin is 5: 100: 150: 20: 30: 12; the mass ratio of the nano powder to the isolating layer precursor is 75: 100.
The invention also discloses a preparation method of the substrate for the terahertz wave detector, which comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) sequentially coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on a heat-resistant substrate to obtain a substrate; after each application, it was dried at room temperature.
The invention also discloses a preparation method of the substrate precursor for the terahertz wave detector, which comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) the substrate precursor for the terahertz wave detector comprises an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor.
The invention also discloses a product obtained by the preparation method.
The mass concentration of potassium hydroxide in the potassium hydroxide methanol solution is 4.5 percent; the molecular weight of the polyvinyl alcohol is 1500-2000. According to the invention, the hydrogen peroxide and the iron tetraphenylporphyrin are added while the polyvinyl alcohol is added, so that the surface activity of the nano powder is increased, more importantly, the molecular weight of the polyvinyl alcohol is reduced, namely, a certain degradation effect is provided for a molecular chain of the polyvinyl alcohol, so that the key help is provided for improving the dispersion performance and the continuity performance of metal oxides after the subsequent conductive nano powder is mixed with resin, especially the influence of the polyvinyl alcohol on the overall performance is avoided, the advantages that the activity of the polyvinyl alcohol is improved by combining other compounds on the surface of the conductive powder and the compatibility is increased are fully exerted, the good electrical performance is reflected, and the sintering effect in the epitaxial preparation process is increased.
In the invention, the thicknesses of the isolating layer precursor, the reinforcing layer precursor and the supporting layer precursor on the heat-resistant substrate are respectively 50 micrometers, 500 micrometers and 260 micrometers; in the process of epitaxial preparation of gallium and nitrogen, each layer is obviously changed to generate chemical reaction, a precursor of the isolation layer is firstly cured to form a cross-linked structure to embody certain mechanical strength, then carbonization is carried out, nano powder of a precursor of the reinforcing layer and an organic system are interacted to form a network structure, and chemical bond acting force is generated between the nano powder and the upper layer and the lower layer to enable the three layers to be fused into a whole, the subsequent carbonization of the organic layer and the formation of a compact structure of the nano powder are carried out, precursors of the supporting layer are mutually dissolved by oxides to finally form a compact structure, particularly, the compact material is mainly a conductive oxidation compound, and meanwhile, the mechanical strength of the material is improved by graphene, the carbon nano tube and silicon elements contained, so that the material above the material can be supported; the optimal thickness ensures that the obtained substrate has excellent mechanical property and electrical property after being stripped from the heat-resistant substrate and also ensures that the problems of pollution, displacement and the like caused by organic matter flow can not occur in the epitaxial preparation process, so that the prepared device has good surface appearance of a sample, an epitaxial film does not have cracks, and the concentration of the n-type back substrate is lower than 102cm-3。
The invention limits the use amount of each component and process parameters, on one hand, no reference exists before the invention, and no theoretical guidance exists, on the other hand, the preparation process of the heteroplasmon is very critical because the heteroplasmon is especially used for detecting the device, and is the basis of the device performance, and the application value of the device is directly influenced, on the other hand, the substrate prepared under the conditions limited by the invention is used for preparing the device, the obtained technical effect is very good, and particularly, the matching of three layers of materials, namely an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor, not only solves the problem of heterojunction support, but also avoids the defects of the existing substrate such as sapphire, and the substrate has strong mechanical property and good electrical property because of the use of nano powder.
The prior art focuses on structural design, for foundationsFew preparative studies, and a small percentage only on the growth of the heteroplasms. Gallium and nitrogen have high melting points and saturated vapor pressures, and it is difficult to produce bulk single crystals by conventional methods. At present, the gallium-nitrogen growth internationally basically adopts heteroepitaxy preparation, and the gallium-nitrogen material is epitaxially grown on a sapphire substrate, which is a universal method for manufacturing optoelectronic devices; in the process of preparing gallium and nitrogen by MOCVD technology, trimethyl gallium is used as MO source, NH3As N source and with H2And N2Or the mixed gas of the two gases is used as carrier gas, reactants are loaded into the reaction cavity and react at a certain temperature to generate molecular groups of corresponding film materials, and the molecular groups are adsorbed, nucleated and grown on the surface of the substrate to finally form the required epitaxial layer. Because the lattice mismatch and the thermal mismatch of gallium-nitrogen and a sapphire substrate are large, the surface appearance of a grown sample is poor, an epitaxial film has cracks, and the concentration of an n-type background is usually 1018cm-3The above. The selection of the material substrate has great influence on the quality of the epitaxial AlGaN/GaN crystal, and has important influence on the performance and reliability of the device, which is also the main reason that the terahertz wave detector in the prior art is slow to mature.
The existing method for growing AlGaN/GaN on sapphire by adopting a two-step method, namely preparing a buffer layer at a low temperature and then growing the AlGaN/GaN at a high temperature, can slightly improve the growth effect; but the improvement is limited, and causes cost rise, complicated steps and resource consumption, because the first step also needs to be carried out at a high temperature of over 500 ℃, and the key is that if the defects exist in the first step, the second step is seriously influenced, and the effect is not as good as that of the preparation directly on the sapphire. The invention designs an isolation layer on a heat-resistant substrate at normal temperature, coats a reinforcing layer and a supporting layer, and then epitaxially grows AlGaN/GaN at high temperature on the supporting layer in one step, in the growth process, the reinforcing layer and the supporting layer are simultaneously sintered to form a compact structure, so that the AlGaN/GaN can be supported, the problem that the existing substrate is not matched with the GaN can be solved, the isolation layer is a polymer layer, the epitaxial preparation process is decomposed into carbon materials, the carbon materials are integrated with the compact structure under the condition of limited thickness, no action force is exerted on the heat-resistant substrate, the heat-resistant substrate can be peeled off from the heat-resistant substrate, the resistance is low, the heat-resistant substrate has simple effect, only plays a role of early support, can be removed after the growth is finished, and any material with a smooth surface and can bear the epitaxial temperature can be selected.
The material of the invention has the characteristics of wide forbidden band, strong bond forming ionicity, strong spontaneous polarization effect in crystals and the like. Compared with the traditional MESFET device, the HEMTs have higher two-dimensional electron gas concentration which is as high as 1014cm2Also, since electrons in the potential well are spatially separated from the donor impurity, electron mobility is greatly improved, which is manifested as excellent characteristics of a HEMT device having high transconductance, high saturation current, and high cutoff frequency.
The heterojunction manufactured based on the invention can have 5000 cm at normal temperature2High electron mobility of/Vs, which makes it more advantageous in high frequency microwave device fabrication than existing devices; the two-dimensional electron gas has a very high density, typically up to 1014cm2The material is 10 times of that of the existing HEMT, which is mainly because the base material of the invention is a strong polarization material, and a large amount of fixed positive charges are generated on the interface by the spontaneous polarization effect and the piezoelectric polarization effect caused by lattice mismatch, which directly results in the formation of high-surface-density two-dimensional electron gas.
High speed is still a goal of microelectronics; high temperature, high power, radiation resistance and the like are still not well solved. The device has the characteristics of wider energy gap, higher saturated electron rate, larger breakdown voltage, smaller dielectric constant, better heat-conducting property and the like, has more stable chemical property, high temperature resistance and corrosion resistance, and is very suitable for manufacturing anti-radiation, high-frequency, high-power and high-density integrated electronic devices and blue, green and ultraviolet optoelectronic devices; the high-power LED lamp has the advantages of high output power and high cut-off frequency, has bearing capacity to severe working conditions, and is expected to be applied to high-temperature and strong-radiation environments which cannot be met by traditional devices. All of these excellent properties well compensate for the problems of the conventional semiconductor devices due to their inherent disadvantages.
The prior art mainly studies the influence of a heterojunction and an antenna on a device, and the mechanism of the influence on a substrate is not clear, but a person skilled in the art knows that the substrate has a great influence on the device as an important component of the device preparation and structure. Unfortunately, due to too large discipline intersection and electrochemical complexity, the research of basic sapphire and silicon carbide substrates is not separated in the field of detection devices at present, the novel substrate is creatively designed for the preparation of heterojunction, the existing device preparation process is not required to be changed, the obtained product has excellent performance and strong application potential, and the brick is thrown away to lead jade, so that researchers in China are expected to perform multidiscipline intersection, the performance of all aspects of the detection device is improved, the wooden barrel effect is avoided, and the effort is made for the development of the detection device in China.
Detailed Description
In the invention, creativity lies in the preparation of the substrate, the substrate in the prior art is completely overturned, and then further operation is carried out on the substrate, such as preparing an AlGaN/GaN layer on the substrate by an epitaxial method 1100 ℃ (optional metal organic chemical vapor phase epitaxy method, molecular beam epitaxy method or hydride vapor phase epitaxy method); then preparing an active region table top, a gate medium, an ohmic contact window and an electrode, wherein the parameters are designed into the conventional general design; after the heat-resistant substrate is removed, the terahertz wave detector is packaged, and the operation of obtaining the terahertz wave detection device can be carried out according to chip epoxy packaging; the terahertz wave detection device is combined with the support, the computer and the indicator light to obtain the terahertz wave detection system which can be operated according to mechanical design and computer connection. The terahertz wave detection system can be used for accurately and stably detecting the terahertz waves in the environment.
Example one
A preparation method of a terahertz wave detector comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 40000 rpm; the flow rate of the concentrate is 90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) sequentially coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on the cleaned sapphire substrate to obtain a substrate; drying at room temperature after each coating;
(6) preparing an aluminum gallium nitride/gallium nitride layer on a substrate by an epitaxial method; and removing the sapphire, and then preparing an active region table board, a gate dielectric, an ohmic contact window and an electrode, thereby obtaining the terahertz wave detector.
Meanwhile, the substrate obtained in the step (5) is cured at 180 ℃/1 hour, and the Td is up to 476 ℃ through testing; sintering the substrate obtained in the step (5) by utilizing an epitaxial method for empty space to obtain a compact conductive material, wherein the compression strength reaches 141MPa, the bending modulus reaches 6.36Gpa, and the impact strength reaches 29.2KJ/m2Can be completely used as a heterojunction supporting material, and has the volume resistivity of 2.7 omega cm; after an aluminum gallium nitrogen/gallium nitrogen layer is prepared on a substrate by an epitaxial method, an expansion coefficient test is carried out, and the error between a heterojunction layer and the substrate layer is less than 0.2%; may have a width of 5000 cm2High electron mobility of/Vs, high two-dimensional electron gas density, typically up to 1014cm2。
Subjecting the prepared device to 1.0 THz reactionThe test shows that the photocurrent is 3.1nA and the noise equipower is 185pW/Hz at normal temperature0.5The responsivity is 182mA/W, and the response time is 6 ps; under liquid nitrogen, the photocurrent was 3.9nA, and the noise equipower was 26pW/Hz0.5The responsivity is 359mA/W, and the response time is 2 ps; at 80 ℃, the photocurrent was 2.4nA, and the noise equipower was 275pW/Hz0.5The responsivity was 125mA/W and the response time was 9 ps.
The mass ratio of the ammonium hexachloroiridate, the dioctyltin, the aluminum nitrate nonahydrate, the ethanol, the propionic acid, the potassium hydroxide methanol solution, the tert-butyl peroxybenzoate, the manganese acetate, the cobalt nitrate, the water and the samarium trimaran is 15: 45: 38: 150: 80: 50: 3: 20: 30: 100: 2; the mass ratio of the centrifugal precipitate, polyvinyl alcohol, hydrogen peroxide, iron tetraphenylporphyrin, 4-diaminophenylmethane and ethyl orthosilicate is 15: 55: 5: 0.1: 40: 50; the mass ratio of the graphene oxide to the epoxy resin to the acetone to the glyceryl monostearate to the diphenyl silanediol to the paraffin is 5: 100: 150: 20: 30: 12; the mass ratio of the nano powder to the isolating layer precursor is 75: 100; the mass concentration of potassium hydroxide in the potassium hydroxide methanol solution is 4.5 percent; the molecular weight of the polyvinyl alcohol is 1500-2000; the thicknesses of the separation layer precursor, the reinforcing layer precursor and the support layer precursor on the heat-resistant substrate are respectively 50 micrometers, 500 micrometers and 260 micrometers.
Example two
A preparation method of a terahertz wave detector comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the hypergravity treatment is 35000 rpm; the flow rate of the concentrate is 80 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) coating an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor on the cleaned sapphire in sequence to obtain a substrate; drying at room temperature after each coating;
(6) preparing an aluminum gallium nitride/gallium nitride layer on a substrate by an epitaxial method; and removing the sapphire, and then preparing an active region table board, a gate dielectric, an ohmic contact window and an electrode, thereby obtaining the terahertz wave detector.
Meanwhile, curing the substrate obtained in the step (5) at 180 ℃/1 hour, and testing shows that the Td reaches 474 ℃; sintering the substrate obtained in the step (5) by utilizing an epitaxial method for empty space to obtain a compact conductive material, wherein the compression strength reaches 142MPa, the bending modulus reaches 6.34Gpa, and the impact strength reaches 29.3KJ/m2Can be completely used as a heterojunction supporting material, and has the volume resistivity of 2.7 omega cm; after an aluminum gallium nitrogen/gallium nitrogen layer is prepared on a substrate by an epitaxial method, an expansion coefficient test is carried out, and the error between a heterojunction layer and the substrate layer is less than 0.2%; may have a width of 5000 cm2High electron mobility of/Vs, high two-dimensional electron gas density, typically up to 1014cm2。
The prepared device is subjected to 1.0 THz application test, and the photocurrent is 3.0nA and the noise isopower is 187pW/Hz at normal temperature0.5The responsivity is 181mA/W, and the response time is 6 ps; under liquid nitrogen, the photocurrent was 3.9nA, and the noise equipower was 28pW/Hz0.5The responsivity is 357mA/W, and the response time is 2 ps; at 80 ℃, the photocurrent was 2.4nA,the noise equipower is 276pW/Hz0.5The responsivity was 123mA/W and the response time was 9 ps.
The mass ratio of the ammonium hexachloroiridate, the dioctyltin, the aluminum nitrate nonahydrate, the ethanol, the propionic acid, the potassium hydroxide methanol solution, the tert-butyl peroxybenzoate, the manganese acetate, the cobalt nitrate, the water and the samarium trimaran is 15: 45: 38: 150: 80: 50: 3: 20: 30: 100: 2; the mass ratio of the centrifugal precipitate, polyvinyl alcohol, hydrogen peroxide, iron tetraphenylporphyrin, 4-diaminophenylmethane and ethyl orthosilicate is 15: 55: 5: 0.1: 40: 50; the mass ratio of the graphene oxide to the epoxy resin to the acetone to the glyceryl monostearate to the diphenyl silanediol to the paraffin is 5: 100: 150: 20: 30: 12; the mass ratio of the nano powder to the isolating layer precursor is 75: 100; the mass concentration of potassium hydroxide in the potassium hydroxide methanol solution is 4.5 percent; the molecular weight of the polyvinyl alcohol is 1500-2000; the thicknesses of the separation layer precursor, the reinforcing layer precursor and the support layer precursor on the heat-resistant substrate are respectively 50 micrometers, 500 micrometers and 260 micrometers.
Preparing an aluminum gallium nitride/gallium nitride layer by an epitaxial method by adopting the conventional sapphire substrate; then preparing an active region table board, a gate medium, an ohmic contact window and an electrode to obtain the terahertz wave detector, and carrying out 1.0 THz application test, wherein the photocurrent is 2.1nA and the noise isopower is 10nW/Hz at normal temperature0.5The responsivity is 106mA/W, and the response time is 12 ps; under liquid nitrogen, the photocurrent is 2.5nA, and the noise equipower is 1nW/Hz0.5The responsivity is 287mA/W, and the response time is 6 ps; at 80 ℃, the photocurrent is 1.1nA, and the noise equipower is 196nW/Hz0.5The responsivity was 37mA/W and the response time was 58 ps.
Claims (4)
1. A preparation method of a substrate precursor for a terahertz wave detector comprises the following steps:
(1) under the protection of nitrogen, mixing ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol and propionic acid; then refluxing and stirring for 5 minutes, and then adding a potassium hydroxide methanol solution and tert-butyl peroxybenzoate; after reacting for 10 minutes, naturally cooling to room temperature, adding ethyl acetate for coagulation and centrifugation; washing the centrifugal precipitate with water, and dispersing in ethanol to obtain a dispersion system; then adding manganese acetate, cobalt nitrate and water, stirring for 10 minutes, adding samarium tricarbate, and stirring for 1 hour to obtain a precursor of the support layer;
(2) adding polyvinyl alcohol, hydrogen peroxide and tetraphenylporphyrin iron into a dispersion system, stirring for 1 hour at 50 ℃, then adding 4, 4-diaminophenylmethane and ethyl orthosilicate, refluxing and stirring for 10 minutes, and then concentrating to obtain a concentrate with the solid content of 80%; carrying out hypergravity treatment on the concentrate; then freeze-drying to obtain nanometer powder; the rotating speed of the supergravity treatment is 35000-40000 rpm; the flow rate of the concentrate is 80-90 mL/min;
(3) adding acetone into graphene oxide and epoxy resin, refluxing and stirring for 20 minutes, adding glyceryl monostearate and diphenyl silanediol, continuously stirring for 10 minutes, adding paraffin, and stirring for 30 minutes to obtain an isolation layer precursor;
(4) adding the nano powder into the precursor of the isolation layer, stirring for 5 minutes, adding the carbon nano tube, and stirring for 10 minutes to obtain a precursor of the reinforcing layer;
(5) the substrate precursor for the terahertz wave detector comprises an isolation layer precursor, a reinforcing layer precursor and a supporting layer precursor.
2. The method according to claim 1, wherein the mass ratio of ammonium hexachloroiridate, dioctyltin, aluminum nitrate nonahydrate, ethanol, propionic acid, methanolic potassium hydroxide solution, tert-butyl peroxybenzoate, manganese acetate, cobalt nitrate, water, samarium trimarate is 15: 45: 38: 150: 80: 50: 3: 20: 30: 100: 2; the mass ratio of the centrifugal precipitate, polyvinyl alcohol, hydrogen peroxide, iron tetraphenylporphyrin, 4-diaminophenylmethane and ethyl orthosilicate is 15: 55: 5: 0.1: 40: 50; the mass ratio of the graphene oxide to the epoxy resin to the acetone to the glyceryl monostearate to the diphenyl silanediol to the paraffin is 5: 100: 150: 20: 30: 12; the mass ratio of the nano powder to the isolating layer precursor is 75: 100.
3. The method according to claim 1, wherein the mass concentration of potassium hydroxide in the potassium hydroxide methanol solution is 4.5%; the molecular weight of the polyvinyl alcohol is 1500-2000.
4. A substrate precursor for a terahertz wave probe produced by the production method according to claim 1.
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| CN109216500A (en) | 2019-01-15 |
| CN107170854A (en) | 2017-09-15 |
| CN109004060B (en) | 2019-11-05 |
| CN109411563A (en) | 2019-03-01 |
| CN107170854B (en) | 2018-09-25 |
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| CN109004060A (en) | 2018-12-14 |
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