CN117587503A - Method for marking substrate temperature in molecular beam epitaxy - Google Patents
Method for marking substrate temperature in molecular beam epitaxy Download PDFInfo
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- CN117587503A CN117587503A CN202311490778.0A CN202311490778A CN117587503A CN 117587503 A CN117587503 A CN 117587503A CN 202311490778 A CN202311490778 A CN 202311490778A CN 117587503 A CN117587503 A CN 117587503A
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- 239000000758 substrate Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 15
- 229910052785 arsenic Inorganic materials 0.000 claims description 57
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 57
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 32
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 20
- 230000007704 transition Effects 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000097 high energy electron diffraction Methods 0.000 claims description 3
- 238000002128 reflection high energy electron diffraction Methods 0.000 claims 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 7
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 239000011733 molybdenum Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- -1 superlattices Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K13/00—Thermometers specially adapted for specific purposes
-
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
Abstract
The invention relates to a method for marking the substrate temperature in molecular beam epitaxy, which can accurately control the substrate temperature in the molecular beam epitaxy, can measure the actual temperature of the substrate under the condition of thermocouple failure of a sample holder, and has important practical application value for the molecular beam epitaxy, especially for materials with narrower growth temperature interval.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for marking the temperature of a substrate in molecular beam epitaxy.
Background
MBE is ultrahigh vacuum equipment, and elemental elements are mainly deposited on the surface of a substrate layer by layer in an ultrahigh vacuum environment in a mode of evaporating the elemental elements from a source furnace to generate molecular beams, so that the growth and preparation of epitaxial materials are realized. The MBE has low growth speed, can realize atomic deposition speed, is beneficial to the preparation of a novel structure, and can greatly reduce the unintended doping of impurities in the epitaxial process by ultrahigh vacuum and improve the quality and purity of the material. Therefore, the method has obvious advantages in the development of novel semiconductor structures such as monoatomic layers, short-period digital alloys, superlattices, quantum dots, nanowires and the like.
Substrate temperature is one of the key parameters in molecular beam epitaxy that require precise control. First, the substrate temperature is too low and the heated atoms or molecules do not migrate and react sufficiently at the substrate surface; conversely, atoms, especially molecules, reaching the substrate at too high a temperature are very susceptible to desorption and even non-stoichiometric films. The proper substrate temperature plays a decisive role in important physical parameters such as surface reconstruction of the substrate, migration distance of surface atoms or molecules, residence time of the surface atoms or molecules and the like, and also influences the components of the growing film. In addition, different growth materials in molecular beam epitaxy have proper growth temperature intervals. Thus, precise control of the substrate temperature is critical to molecular beam epitaxy.
Molecular beam epitaxy equipment typically provides a sample holder for a substrate with heater wires and thermocouples to achieve heating control under temperature feedback. The temperature measured by the thermocouple is fed back to a temperature control system, and the temperature control system regulates and controls heating power according to parameters such as a feedback temperature value, a target temperature set value, a heating rate and the like. However, the difference of the substrate materials, the size of the molybdenum support and the service time can cause deviation of the feedback temperature measured by the thermocouple and the actual substrate temperature, thereby affecting the crystal growth quality. Thus, accurate measurement and regulation of substrate temperature is a primary premise for achieving high quality crystal growth.
From the above, it can be seen that the substrate temperature is a critical parameter in molecular beam epitaxy, and that control of the substrate temperature depends on thermocouple readings and heater wire power, which is highly ambiguous. At present, the prior art still lacks of accurate regulation and control on the temperature of a substrate.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for marking the substrate temperature in molecular beam epitaxy, which can accurately regulate and control the substrate temperature in the molecular beam epitaxy and has important practical application value for growing III-V materials, especially materials with narrower growth temperature intervals in the molecular beam epitaxy.
The invention discloses a method for marking the temperature of a substrate in molecular beam epitaxy, which comprises the following steps:
(1) Measuring beam current of the arsenic source furnace under different valve openings in a vacuum environment, and drawing a beam current-valve opening curve of the arsenic source furnace; (2) Measuring the temperature of the surface reconstruction of the substrate under the valve opening of the arsenic source furnace when the surface reconstruction is converted, and drawing a valve opening-conversion temperature curve; (3) Determining the surface reconstruction transition temperature of the substrate under different arsenic beam sizes according to the valve opening-transition temperature curve of the step (2) and the beam-valve opening curve of the arsenic source furnace of the step (1), so as to obtain an arsenic beam-transition temperature curve;
(4) And calibrating the surface temperature of the substrate through an arsenic beam current-transition temperature curve.
The preferred mode of the method is as follows:
and (3) measuring the beam current of the arsenic source furnace under different valve openings by adopting a beam current gauge in the step (1).
The opening degree of the valve in the step (1) is 20-100%.
The opening degree of the valve in the step (2) is 20-100%.
And (3) setting the valve opening in the steps (1) and (2) to be the valve opening gradient, wherein the valve opening gradient in the step (1) and the valve opening gradient in the step (2) are the same.
The substrate in the step (2) is a gallium arsenide (001) substrate.
The surface of the substrate in the step (2) is a gallium arsenide (001) surface.
The substrate surface reconstruction transition temperature is observed and recorded by high energy electron diffraction RHEED in step (2).
Temperature at which the surface reconstruction of the substrate in step (2) is transformed: the substrate surface in the case of a fixed arsenic beam reconfigures from (2×4) to c (4×4) when the temperature changes from high to low.
The construction of the valve opening-transition temperature curve in the step (2) specifically comprises the following steps: and (3) transferring the substrate into molecular beam epitaxy equipment, heating, starting arsenic protection, observing that the surface of the substrate is reconstructed into (2 multiplied by 4) through RHEED after deoxidation is finished, reducing the temperature of the substrate after setting the valve opening of an arsenic source furnace, and when the temperature of the substrate reaches T1, converting the surface reconstruction of the substrate into c (4 multiplied by 4) from (2 multiplied by 4), wherein T1 is the conversion temperature of the substrate in arsenic beam, and repeating the steps to measure the substrate conversion temperatures under different valve openings to obtain a valve opening-conversion temperature curve.
In the step (4), the temperature of the surface of the substrate is calibrated through an arsenic beam-transition temperature curve, specifically, when the size of the arsenic beam is determined by taking the established arsenic beam-transition temperature curve as a standard, the temperature corresponding to the temperature when the reconstruction of the surface of the substrate is changed can be read out according to the arsenic beam-transition temperature curve instead of thermocouple feedback temperature, so that the influence of different machine thermocouples and molybdenum supports on the temperature of the substrate can be avoided. Thus realizing the calibration of the substrate temperature.
The method is applied to the molecular beam epitaxy growth of III-V materials.
The invention aims to establish a quantitative relation between the substrate temperature and the arsenic beam, and the calibrated substrate temperature can be calculated by utilizing the arsenic beam measured by a beam gauge. The relationship is established according to the correspondence between the gallium arsenide (001) surface reconstruction transition point and the arsenic beam current.
The III-V compound material has excellent optical performance due to the semiconductor characteristic of a direct band gap, is a key of future photoelectronic technology, and particularly plays a key role in the fields of optical fiber communication, space detection and the like as a light source and a detector based on an arsenide semiconductor material of a gallium arsenide substrate. The accurate control of the substrate temperature is of great importance to the molecular beam epitaxy of high quality crystal thin films and semiconductor devices with excellent research and development performances. Therefore, the method for accurately calibrating the substrate temperature has extremely high application value for enterprise production and scientific research.
In molecular beam epitaxy techniques, the reconstruction of the substrate surface is typically observed in real time by Reflected High Energy Electron Diffraction (RHEED). The substrate surface reconstruction typically changes as the substrate temperature or surface composition changes. Thus, the surface properties of the crystal can be judged by feedback of RHEED pattern. For example, the surface reconstruction of gallium arsenide (001) substrates at higher temperatures is manifested as a (4 x 2) reconstruction of gallium-rich surfaces, with the surface transition from gallium-rich to arsenic-rich surfaces as the substrate temperature decreases, the corresponding surface reconstruction transitioning from (4 x 2) to (2 x 4) or c (4 x 4). The three surface reconstructions are determined by the substrate temperature and the arsenic beam, and when the arsenic beam is fixed, the temperature at which the different surface reconstructions are transformed is unique. Wherein the transition between the (2 x 4) reconstruction and the c (4 x 4) reconstruction is a very rapid and reversible process. Therefore, the reconstruction transition points are measured under different arsenic beam flows, and the substrate surface reconstruction transition temperatures corresponding to different arsenic beam flows can be obtained, so that a function curve between the arsenic beam flows and the substrate temperature is established, and the arsenic beam flows and the substrate temperature in the curve are in one-to-one correspondence.
In the molecular beam epitaxy process, a substrate heater heats the substrate to a specific temperature to ensure epitaxial growth of the crystalline thin film. A common molecular beam epitaxial substrate heater is a thermal radiation heater. Heat is transferred to the substrate primarily by thermal radiation. And detecting the temperature around the inner ring and the outer ring of the heater by a thermocouple, and feeding back to a temperature regulating system. The process can be influenced by different machine models and the service time of the molybdenum support. The thermal conductivity of the molybdenum support can change with time of use, thereby affecting the temperature change of the substrate. Therefore, a fixed method is needed to calibrate the substrate temperature. The temperature of the gallium arsenide substrate surface is calibrated in a mode that the surface reconstruction transition point temperature corresponds to the arsenic beam, so that the influence of molybdenum support state change on the temperature and errors caused by thermocouple measurement can be avoided, and the calibration method is very important for the actual epitaxial growth process.
Advantageous effects
The method establishes a mode for calibrating the substrate temperature, is suitable for MBE equipment of different types, has important practical value for epitaxial growth of III-V group materials by molecular beams, can ensure the repeatability of growth conditions in the production and scientific research processes, and improves the yield and consistency of the growth materials;
when the substrate needs to reach a certain temperature on the curve, the arsenic beam corresponding to the temperature is found according to the curve, the substrate is placed in the arsenic beam atmosphere, the temperature is changed, the substrate is subjected to reconstruction transformation as described above, and the temperature during transformation is the temperature which is required to be reached. If the feedback is based on thermocouple, a lot of errors can occur, the repeatability cannot be ensured, but the method of the invention is not influenced by thermocouple errors and molybdenum holders, and the repeatability and consistency are ensured;
the method can accurately regulate and control the temperature of the substrate in the molecular beam epitaxy, can measure the actual temperature of the substrate under the condition of failure of the thermocouple of the sample holder, and has important practical application value for growing III-V materials in the molecular beam epitaxy, especially materials with narrower growth temperature intervals.
Drawings
FIG. 1 is a beam current versus valve opening curve for an arsenic source furnace at different valve openings according to example 1;
FIG. 2 is a schematic diagram of the reconstruction of the gallium arsenide (001) substrate surface c (4X 4) of example 1;
FIG. 3 is a schematic diagram of the reconstruction of the gallium arsenide (001) substrate surface (2X 4) of example 1;
FIG. 4 is a graph of gallium arsenide (001) substrate valve opening versus transition temperature for example 1;
FIG. 5 is a plot of the different arsenic beam sizes versus the temperature of the surface reconstruction transition point of the gallium arsenide (001) substrate of example 1.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1
The embodiment provides a method for marking the temperature of a substrate in molecular beam epitaxy, which comprises the following steps:
(1) Measuring beam current-valve opening curves of the arsenic source furnace under different valve openings by using a beam current gauge in a vacuum environment;
(2) Measuring the temperature of gallium arsenide (001) surface reconstruction transition under different arsenic source furnace valve opening degrees, and drawing a valve opening degree-transition temperature curve;
(3) Determining the surface reconstruction transition temperature of the gallium arsenide under different arsenic beam sizes according to the valve opening-transition temperature curve and the beam-valve opening curve of the arsenic source furnace, and drawing an arsenic beam-transition temperature curve;
(4) And measuring the surface reconstruction transition temperature of the gallium arsenide under the fixed arsenic beam current, and measuring the accurate substrate temperature at the moment according to the arsenic beam current-transition temperature curve.
Specifically, gallium arsenide (001) is used as a substrate sample in this embodiment, and is placed in a molecular beam epitaxy apparatus for testing. Firstly, under a good vacuum environment, beam current-valve opening curves of an arsenic source furnace under different valve openings are measured through a beam current gauge, as shown in fig. 1.
And then the gallium arsenide substrate is conveyed into a molecular beam epitaxy device, the gallium arsenide substrate is heated by a heater, arsenic protection is started after the temperature reaches 400 ℃, the surface reconstruction of the gallium arsenide substrate is observed to be (2 multiplied by 4) through RHEED after deoxidation is finished, the temperature of the substrate is reduced after the valve opening of the arsenic source furnace is set, and when the temperature of the substrate reaches a certain point, the surface reconstruction of the substrate is converted from (2 multiplied by 4) to c (4 multiplied by 4) (shown in fig. 2 and 3), and the point is the conversion temperature of the substrate in arsenic beam. This step is repeated to measure the substrate transition temperature at different valve openings and to establish a valve opening-transition temperature curve, as shown in fig. 4. A curve between arsenic beam and transition temperature can be established from the relationship between the valve opening and arsenic beam in fig. 1 and the relationship between the valve opening and the substrate transition temperature in fig. 4, as shown in fig. 5.
When the molybdenum support needs to be replaced or used for a long time, the transformation temperature of the surface reconstruction of the gallium arsenide substrate can be tested through the steps under the condition of fixing the beam current of the arsenic source furnace, and the actual temperature of the surface of the substrate is calibrated by referring to FIG. 5.
Claims (10)
1. A method of identifying a substrate temperature in molecular beam epitaxy, comprising:
(1) Measuring beam current of the arsenic source furnace under different valve openings in a vacuum environment, and drawing a beam current-valve opening curve of the arsenic source furnace;
(2) Measuring the temperature of the surface reconstruction of the substrate under the valve opening of the arsenic source furnace when the surface reconstruction is converted, and drawing a valve opening-conversion temperature curve;
(3) Determining the surface reconstruction transition temperature of the substrate under different arsenic beam sizes according to the valve opening-transition temperature curve of the step (2) and the beam-valve opening curve of the arsenic source furnace of the step (1), so as to obtain an arsenic beam-transition temperature curve;
(4) And calibrating the surface temperature of the substrate through an arsenic beam current-transition temperature curve.
2. The method of claim 1, wherein the beam gauge is used in step (1) to measure the beam current of the arsenic source furnace at different valve openings.
3. The method of claim 1, wherein the valve opening in steps (1) and (2) is 20-100%.
4. The method according to claim 1, wherein the valve opening in the steps (1) and (2) is a valve opening gradient setting, and the valve opening gradient setting in the steps (1) and (2) is the same.
5. The method of claim 1, wherein the substrate in step (2) is a gallium arsenide (001) substrate.
6. The method of claim 1, wherein the substrate surface in step (2) is a gallium arsenide (001) surface.
7. The method of claim 1, wherein the substrate surface reconstruction transition temperature is observed and recorded in step (2) by high energy electron diffraction RHEED.
8. The method of claim 1, wherein the temperature at which the surface reconstruction of the substrate in step (2) is changed is: the substrate surface in the case of a fixed arsenic beam reconstructs the temperature at which it changes from (2×4) to c (4×4) when the temperature changes from high to low.
9. The method according to claim 1, wherein the valve opening-transition temperature curve in step (2) is constructed specifically as follows: and (3) transferring the substrate into molecular beam epitaxy equipment, heating, starting arsenic protection, observing that the surface of the substrate is reconstructed into (2 multiplied by 4) through RHEED after deoxidation is finished, reducing the temperature of the substrate after setting the valve opening of an arsenic source furnace, and when the temperature of the substrate reaches T1, converting the surface reconstruction of the substrate into c (4 multiplied by 4) from (2 multiplied by 4), wherein T1 is the conversion temperature of the substrate in arsenic beam, and repeating the steps to measure the substrate conversion temperatures under different valve openings to obtain a valve opening-conversion temperature curve.
10. Use of the method of claim 1 for the molecular beam epitaxy of group III-V materials.
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| CN202311490778.0A CN117587503A (en) | 2023-11-10 | 2023-11-10 | Method for marking substrate temperature in molecular beam epitaxy |
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| CN202311490778.0A CN117587503A (en) | 2023-11-10 | 2023-11-10 | Method for marking substrate temperature in molecular beam epitaxy |
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