CN111334760A - Method for preparing atomic layer thermopile film on polycrystalline or amorphous substrate - Google Patents
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- 239000000758 substrate Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000007735 ion beam assisted deposition Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims 3
- 239000010408 film Substances 0.000 abstract description 31
- 239000013078 crystal Substances 0.000 abstract description 21
- 239000010409 thin film Substances 0.000 abstract description 9
- 238000012360 testing method Methods 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 238000010884 ion-beam technique Methods 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000008020 evaporation Effects 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 24
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 22
- 239000000395 magnesium oxide Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 7
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 5
- 229910000856 hastalloy Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 2
- 229910003097 YBa2Cu3O7−δ Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000007274 generation of a signal involved in cell-cell signaling Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/34—Sputtering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
- G01J5/12—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors using thermoelectric elements, e.g. thermocouples
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- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
- G01J5/12—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors using thermoelectric elements, e.g. thermocouples
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Abstract
The invention belongs to the technical field of film preparation, and particularly relates to a method for preparing an atomic layer thermopile film on a polycrystalline or amorphous substrate. The invention adopts IBAD method to obtain biaxial texture on the amorphous substrate; and by changing the included angle between the incident direction of the ion beam and the incident direction of the MgO evaporation source which are commonly used and relative to the substrate, the film forms a structure similar to the inclined single crystal surface with the c axis inclined to the normal of the substrate, and finally the film with the inclined crystal grains of the c axis is obtained. The invention is suitable for polycrystalline and amorphous surfaces, can not only use a metal strip with thin thickness, high flexibility and good thermal conductivity to replace a single crystal in the prior art as a substrate, but also can be applied to directly deposit a thin film on the surface of a tested piece to manufacture an integrated atomic layer thermopile sensor, and provides a brand new technical means for heat flow testing of a complex-shaped surface.
Description
Technical Field
The invention belongs to the technical field of film preparation, and particularly relates to a method for preparing an Atomic layer thermopile film on a polycrystalline or amorphous substrate, which is applied to preparing the Atomic layer thermopile (Atomic layer thermopile) film on a metal substrate or a composite material.
Background
An atomic layer thermopile is a thin film structure with thermoelectric anisotropy. High temperature superconducting materials, e.g. YBa2Cu3O7-δ(YBCO) and the like have an alternating layered structure of a plurality of metal elements: wherein CuO2The layer conductivity is high and the Y (Ba) -O layer conductivity is low. In some non-layered conductive materials, the materials can also have certain conductivity anisotropy by using methods such as strain control and the like. After the material with conductivity anisotropy is prepared into a state that the epitaxial growth c axis is obliquely oriented, under the condition of heat flow in the depth direction, the upper surface and the lower surface of the film material form temperature difference, and a large number of thermocouples which are connected in series and are just like two materials with different conductivities are formed on the upper surface and the lower surface of the film material. Due to the thin film thickness, a large number of thermocouple junctions (up to 10A) are included in small-sized films6/cm) and is therefore referred to as an atomic layer thermopile. The small voltages output by each atomic layer thermocouple under thermal shock are added together to form a larger thermopile output voltage signal. Since heat absorption and diffusion occur in a thin film of nanometer order thickness, the heat capacity is very small, the signal generation is caused by temperature difference, and there is no need to establish thermal equilibrium, so the response speed is fast.
In order to achieve tight orientation control for the tilted growth of anisotropic conductive films, atomic layer thermopile thermal flow sensors are typically fabricated on a single crystal surface that is beveled at an angle. The film epitaxially grown on the single crystal substrate has high orientation consistency and a certain inclination angle, and the characteristics of the film are easy to control. In the research of unsteady heat conduction phenomena, such as the inner surface of an engine, turbine blades, the boundary layer of an aircraft, the irregularly-shaped turbulent flow boundary layer and the like, the ultrahigh-speed flow has high requirements on the sensitivity (voltage output/heat flux density) and the time response (so as to achieve a large signal-to-noise ratio at high frequency) of the sensor, and the atomic layer thermopile heat flow sensor with small volume, fast response and wide range is expected to have good application. In the application scenes, however, the problem that the independent sensor made of single crystal is not easy to mount in the measurement is generated due to the high-speed motion of the measured piece and the impact of high-speed heat flow on the surface; moreover, the hard and brittle characteristics of single crystals cannot meet the application requirements of non-planar application occasions: because the deformation is very small, the single chip can not be effectively attached to the surface of the tested piece to form a surface which interferes the flow of the fluid; in addition, the thickness of the single crystal is large and the heat conduction characteristic is inconsistent with the measured piece, so that the heat transfer variation of the single crystal is greatly different from that of the measured piece, and additional test errors can be caused.
Therefore, if an atomic layer thermopile heat flow sensor with thin thickness, high flexibility and good heat conductivity can be developed, the application field of the atomic layer thermopile heat flow sensor can be greatly expanded. Particularly, the atomic layer thermopile heat flow sensor with the heat flow test function can be directly prepared on the surface of a tested piece, and a brand new technical means is provided for the heat flow test of the surface with a complex shape.
Disclosure of Invention
In order to solve the problems and realize the preparation of the atomic layer thermopile film on the surface of a polycrystalline or amorphous tested piece or a very thin flexible metal substrate, the invention provides a method for preparing the atomic layer thermopile film on the polycrystalline or amorphous substrate.
A method for preparing an atomic layer thermopile film on a polycrystalline or amorphous substrate comprises the following specific steps:
step 1, carrying out planarization treatment on the surface of a substrate, wherein the surface root mean square Roughness (RMS) is less than or equal to 2nm, and the substrate is polycrystalline or amorphous;
and 2, preparing the MgO film with the thickness of 10-20nm on the substrate surface subjected to the planarization treatment in the step 1 by using an IBAD method, wherein the ion incidence direction and the MgO particle incidence direction are in the same plane, and the included angle between the ion incidence direction and the MgO particle incidence direction is kept at 40-55 degrees.
And 3, extending a MgO film with the thickness of 100-. So as to improve the texture of the MgO film and improve the surface flatness and provide a good foundation for preparing the atomic layer thermopile functional layer on the MgO film.
Step 4, growing YBa with the thickness of 50-500nm on the surface treated by the epitaxial MgO film in the step 32Cu3O7-δA film.
Further, the step 1 is to process the polycrystalline or amorphous surface with larger surface roughness by a polishing or solution deposition planarization method: since high-quality ion beam assisted electron beam evaporation magnesium oxide (IBAD-MgO) thin films are grown, substrates providing nanoscale flatness are required.
According to the invention, an IBAD method is adopted to obtain a biaxial texture (similar to a single crystal and small included angle between crystal grains) on an amorphous substrate, and MgO is a material for quickly forming the biaxial texture (the thickness of 10nm is optimal); and by changing the included angle between the incident direction of the ion beam and the incident direction of the MgO evaporation source which are commonly used and relative to the substrate, the film forms a structure similar to the inclined single crystal surface with the c axis inclined to the normal of the substrate, and finally the film with the inclined crystal grains of the c axis is obtained.
In conclusion, the IBAD-MgO technology adopted by the invention can obtain a c-axis inclined structure which is similar to the inclined cutting surface of a single crystal atomic layer thermopile sensor; the method used by the whole technical route is suitable for polycrystalline and amorphous surfaces, can not only use a metal strip with thin thickness, high flexibility and good thermal conductivity to replace a single crystal in the prior art as a substrate, but also can be applied to directly depositing a thin film on the surface of a tested piece to manufacture an integrated atomic layer thermopile sensor, and provides a brand new technical means for heat flow testing of a complex-shaped surface.
Drawings
FIG. 1 is a schematic diagram showing the relative positions of the sample substrate and the incident direction of the ion incident and evaporated MgO particles in the preparation of an IBAD-MgO thin film.
Fig. 2 is a schematic view of the sample mounting when measuring the laser induced electrical signal.
Fig. 3, laser induced electrical signal response of the sample.
FIG. 4, (a) XRD-2 θ scan of the sample; (b) XRD-omega scanning of a MgO (002) crystal face of a sample; (c) XRD-omega scanning of the crystal face of sample YBCO (006).
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example (b):
preparing a thermoelectric anisotropy YBa with a structure that the c axis is inclined to the normal on a Hastelloy base band, wherein the size of the thermoelectric anisotropy YBa is 2mm x10 mm2Cu3O7-δA film.
Step 1, polishing or preparing a solution deposition planarization coating on a Hastelloy (Hastelloy C-276) base band, wherein the root mean square Roughness (RMS) of the surface of 5 mu m x5 mu m is less than 2 nm. It was cut to a size of 10mm x10 mm as the sample base.
And 2, growing a 10nm IBAD-MgO film on the substrate. Referring to FIG. 1, n is the normal of the substrate, and the incident direction of MgO particles and the incident direction of the ion beam are in the same plane, which is perpendicular to the substrate. The incidence angle of MgO particles is 40 degrees, the incidence angle of ion beams is 5 degrees, and the included angle between the two angles is 45 degrees. Initial pressure 4x 10 in experiment-4Adding Ar under Pa to make the working pressure of the ion source be 2.8x 10-2Pa; the energy of the ion beam is 800eV, and the beam current is 120 mA; MgO deposition rate was 0.25 nm/s.
And 3, extending a 120nm MgO film on the surface subjected to IBAD-MgO treatment. Initial pressure 4x 10 in experiment- 4Pa, adding O2Air pressure of 2.8x 10-2Pa, and the heating temperature of the substrate is 600 ℃.
Step 4, growing 300nm YBa by using a magnetron sputtering method after extending MgO2Cu3O7-δFilm, sample cut to size 2mm x10 mm.
And 5, using resistance evaporation Ag films at two ends of the strip-shaped sample as electrodes for testing.
The prepared sample is subjected to laser induced electrical signal and XRD test, and the result is as follows:
the sample was mounted as shown in fig. 2, with a pulsed laser incident normal to the sample surface to create a thermal gradient across the sample top and bottom surfaces, illuminating an area of 2mm x 2mm, total energy per time of 0.4mJ, spaced 20ns apart.
The response signal obtained by connecting both ends of the electrode with an Oscilloscope (Agilent Digital Storage Oscilloscope 7052A) is defined as 1/e of the peak value as shown in FIG. 3, and the intersection point of the horizontal line of the attenuation value and the signal is the start point and the end point of the rise and the fall of the response. The signal peak time is 0. Signal peak 330mV, rising edge response time 55ns, falling edge response time 170 ns. The sample shows the thermoelectric anisotropy of the atomic layer thermopile thin film, and has obvious signal response and short response time under the thermal gradient.
The sample was subjected to 2 theta and omega scans of XRD. From the 2 θ scan in fig. 4(a), the MgO (002) peak θ becomes 21.53 °, and the YBCO (006) peak θ becomes 23.35 °.
As shown in the ω scan of the MgO (002) crystal plane in fig. 4(b), the ω scan peak is 22.6 ° and shifted from the center by 1.07 ° (θ is 21.53 °, and 22.6 ° to 21.53 ° is 1.07 °).
As shown by the ω scan of the YBCO (006) crystal plane of fig. 4(c), the ω scan peaks 25 ° off-center by 1.65 ° (θ is 25 °,25 ° -23.35 ° -1.65 °).
The MgO of the sample of the embodiment has a structure that the c-axis is inclined to the normal line of the substrate, and the YBCO grown on the basis of the structure also has a structure that the c-axis is inclined to the normal line of the substrate; the laser induced electrical signal shows that the film has a thermoelectric anisotropy derived from such a c-axis tilted structure; the sample has obvious signal response and short response time under the thermal gradient.
In conclusion, the successful application of the invention on the metal base band shows that the technical route is suitable for the surfaces of polycrystal and amorphous, not only can use a metal strip to replace single crystal as a substrate, but also can be applied to directly deposit a thin film on the surface of a tested piece to manufacture an integrated atomic layer thermopile sensor, solves the difficulty of the existing independent single crystal sensor in installation and measurement, and provides a brand new technical means for the heat flow test of the surface with a complex shape.
Claims (3)
1. A method for preparing an atomic layer thermopile film on a polycrystalline or amorphous substrate comprises the following specific steps:
step 1, carrying out planarization treatment on the surface of a substrate, wherein the surface root mean square roughness RMS is less than or equal to 2nm, and the substrate is polycrystalline or amorphous;
step 2, preparing a MgO film with the thickness of 10-20nm on the substrate surface subjected to the planarization treatment obtained in the step 1 by using an IBAD method, wherein the ion incidence direction and the MgO particle incidence direction are in the same plane, and the included angle between the ion incidence direction and the MgO particle incidence direction is kept at 40-55 degrees;
step 3, extending a MgO film with the thickness of 100-;
step 4, growing YBa with the thickness of 50-500nm on the surface treated by the epitaxial MgO film in the step 32Cu3O7-δA film.
2. The method of preparing an atomic layer thermopile film on a polycrystalline or amorphous substrate of claim 1, wherein: the step 1 treats the surface roughness by a polishing or solution deposition planarization method.
3. The method of preparing an atomic layer thermopile film on a polycrystalline or amorphous substrate of claim 1, wherein: the included angle between the incident ions and MgO particles in the IBAD method is 45 degrees.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114136501A (en) * | 2021-11-26 | 2022-03-04 | 山东大学 | Thin film type heat flow sensor structure and metal electrode preparation method thereof |
CN114910183A (en) * | 2022-03-28 | 2022-08-16 | 电子科技大学 | Atomic layer thermopile heat flow sensor and preparation method |
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CN104810468A (en) * | 2015-04-28 | 2015-07-29 | 苏州新材料研究所有限公司 | Preparation method for dual spindle texture high-temperature superconductive buffer layer |
CN105705921A (en) * | 2013-07-17 | 2016-06-22 | 相干公司 | Laser power and energy sensor utilizing anisotropic thermoelectric material |
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CN105705921A (en) * | 2013-07-17 | 2016-06-22 | 相干公司 | Laser power and energy sensor utilizing anisotropic thermoelectric material |
CN104810468A (en) * | 2015-04-28 | 2015-07-29 | 苏州新材料研究所有限公司 | Preparation method for dual spindle texture high-temperature superconductive buffer layer |
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Title |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114136501A (en) * | 2021-11-26 | 2022-03-04 | 山东大学 | Thin film type heat flow sensor structure and metal electrode preparation method thereof |
CN114910183A (en) * | 2022-03-28 | 2022-08-16 | 电子科技大学 | Atomic layer thermopile heat flow sensor and preparation method |
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