CN117518226A - Method for marking arsenic source furnace beam current size in molecular beam epitaxy - Google Patents
Method for marking arsenic source furnace beam current size in molecular beam epitaxy Download PDFInfo
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- CN117518226A CN117518226A CN202311337911.9A CN202311337911A CN117518226A CN 117518226 A CN117518226 A CN 117518226A CN 202311337911 A CN202311337911 A CN 202311337911A CN 117518226 A CN117518226 A CN 117518226A
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 70
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 230000007704 transition Effects 0.000 claims abstract description 34
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims abstract description 26
- 230000009466 transformation Effects 0.000 claims abstract description 4
- 238000002474 experimental method Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000000097 high energy electron diffraction Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 16
- 239000000956 alloy Substances 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002128 reflection high energy electron diffraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
- C30B25/165—Controlling or regulating the flow of the reactive gases
-
- 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
- C30B29/42—Gallium arsenide
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/29—Measurement performed on radiation beams, e.g. position or section of the beam; Measurement of spatial distribution of radiation
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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
The invention relates to a method for marking the beam current of an arsenic source furnace in molecular beam epitaxy, which comprises the following steps: measuring beam values under different arsenic valve sizes; (2) Testing the temperature of the surface of the gallium arsenide substrate when the reconstruction transformation phenomenon occurs by using different arsenic beams, and establishing a relation curve of the arsenic beams and the reconstruction transformation temperature; (3) determining the beam value of arsenic according to the temperature of the reconstruction transition. The invention can accurately obtain the accurate value of the arsenic beam current in the molecular beam epitaxy, and has important practical application value for the molecular beam epitaxy, especially for the alloy growth requiring two V-group sources.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for marking the beam current of an arsenic source furnace in molecular beam epitaxy.
Background
The Molecular Beam Epitaxy (MBE) technology is a general technology for epitaxially growing semiconductor, metal and insulator films, and is a novel semiconductor microstructure material meeting specific requirements can be prepared by the molecular beam epitaxy technology through precisely controlling beam flux and deposition conditions by heating evaporation source materials to generate molecular beams and depositing molecules or atoms layer by layer on a substrate under ultrahigh vacuum conditions.
One of the key parameters in molecular beam epitaxy techniques that require precise control is the sample growth temperature. First, the sample temperature determines the physical parameters of the surface reconstruction of the sample, the migration length of molecules/atoms on the surface and the residence time thereof, and also determines the crystal quality during the growth process. The epitaxial growth of the crystal film is required to be carried out in an optimized temperature range. Therefore, measurement and accurate control of the sample temperature is critical. In general, in a molecular beam epitaxy device, a Thermocouple (TC) is installed on a sample frame to measure the temperature, a temperature signal measured by the Thermocouple is input into a temperature control system, and the output power of a heating power supply is adjusted to control the temperature of a sample.
Another key parameter in molecular beam epitaxy techniques that requires precise control is the molecular beam current that is supplied to the crystal growth. The molecular/atomic beam is the raw material for epitaxial growth of crystal film, and the size of the beam directly determines the growth speed and quality of the film. For a multi-element compound or alloy material, the supply ratio of the different elements is very critical, and the element composition of the material is determined. For example, the beam sizes of indium and gallium directly determine the component ratio of indium and gallium, and in addition, excessive arsenic beam needs to be supplied to obtain high-quality InGaAs crystal materials. Therefore, measurement and control of beam current in molecular beam epitaxy is also very important. Typically, molecular beam epitaxy measures vacuum by moving an ion gauge to the center of the sample holder, this value is called beam, also called beam equivalent pressure (Beam equivalent pressure). This ion gauge is known as a beam gauge in a molecular beam epitaxy apparatus for measuring the molecular/atomic beam size.
From the above, it can be seen that two key parameters in molecular beam epitaxy technology, namely temperature and beam current, are measured independently by different physical principles and hardware components. There is currently no study in the prior art concerning the link between the two key parameters mentioned above.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for calibrating the beam current of an arsenic source furnace in molecular beam epitaxy, which can accurately obtain the accurate value of the arsenic beam current in the molecular beam epitaxy and has important practical application value for the growth of the molecular beam epitaxy, especially the alloy requiring two V-group sources.
The invention provides a method for marking the beam current of an arsenic source furnace in molecular beam epitaxy, which comprises the following steps:
(1) Under the condition of good vacuum background, a beam monitor is started, the corresponding beam sizes of the arsenic source furnace under different valve openings are measured, and a valve opening-arsenic beam curve is drawn;
(2) Regulating the valve opening of the arsenic source furnace, measuring the corresponding transition point temperature when the surface reconstruction phenomenon of the gallium arsenide sample occurs, and drawing a transition point temperature-valve opening curve;
(3) Determining the arsenic beam size corresponding to the gallium arsenide sample surface transition point temperature in the experiment according to the transition point temperature-valve opening curve and the valve opening-arsenic beam curve, and drawing the transition point temperature-arsenic beam curve;
(4) For unknown arsenic beam, measuring the temperature of the transition point of the surface reconstruction of the gallium arsenide sample, and measuring the size of the arsenic beam at the moment according to the curve of the temperature of the transition point and the arsenic beam.
And (3) determining the surface transition point temperature of the gallium arsenide sample by using high-energy electron diffraction in the step (2).
The reconstruction phenomenon in the step (2) refers to the transformation of the surface reconstruction of the gallium arsenide sample from (2×4) to c (4×4).
The invention aims to establish a quantitative relation between the substrate temperature and the arsenic beam, and the arsenic beam value under specific conditions can be calculated by measuring the substrate temperature by utilizing a thermocouple. This quantitative relationship is established by measuring the surface reconstruction transition point of the gallium arsenide (001) surface.
In molecular beam epitaxy techniques, the reconstruction of the substrate surface is generally observed by Reflection High Energy Electron Diffraction (RHEED), the surface reconstruction reacting the physicochemical characteristics of the sample surface. When the temperature of the sample or the elemental composition of the surface changes, typically the surface reconstruction of the sample changes. Thus, a basic determination of the crystal surface properties can be made by observing the RHEED pattern. For example, gallium-rich surface of gallium arsenide in the molecular beam epitaxy process shows a (4×2) reconstruction pattern, when the arsenic beam is enlarged, the surface is converted into an arsenic-rich surface, and the (2×4) or c (4×4) surface reconstruction is respectively shown at different sample temperatures, which correspond to the surface state of the arsenic-rich surface. The three reconstructions of the gallium arsenide (001) surface can be transformed, and the reconstruction of the surface is determined by the substrate temperature and the arsenic beam. In particular, the transition between the (2 x 4) and c (4 x 4) reconstructions is very rapid and reversible. The temperature of the substrate and the arsenic beam are closely related under the condition that the reconstruction transition point is located. Therefore, by measuring the reconstruction transition points at different substrate temperatures, the arsenic beam current value corresponding to the set substrate temperature can be obtained, so that a corresponding curve between the substrate temperature and the arsenic beam current is established, wherein the substrate temperature and the arsenic beam current in the curve are in one-to-one correspondence, and a monotonic function is formed between the substrate temperature and the arsenic beam current.
In the molecular beam epitaxial growth process, the arsenic source furnace is in a use state, the mass of arsenic raw materials in the crucible is continuously reduced, the distribution state in the crucible is changed, and meanwhile, the state of a source furnace valve is slightly changed along with time, so that the size of arsenic beam is changed. Therefore, the arsenic beam needs to be measured periodically. For the traditional method of testing by using a beam gauge, measuring the arsenic beam by using the temperature of the surface reconstruction transition point is a very important supplementary method.
The III-V compound material has excellent optical and electrical properties, is widely used for manufacturing novel semiconductor photoelectric material devices, particularly an arsenide semiconductor material based on a gallium arsenide substrate, has important application in visible light and near infrared band photoelectric devices, and is also applied to high-speed radio frequency devices. Accurate measurement and control of arsenic beam size is of great importance for the fabrication of semiconductor devices with excellent performance using molecular beam epitaxy techniques. Therefore, the method for accurately calibrating the arsenic beam current so as to realize the accurate control of the sample growth conditions is found to have important value for scientific research and enterprise production.
Advantageous effects
The method can accurately obtain the accurate value of the arsenic beam in the beam epitaxy, has certain universality, is not influenced by equipment types, has important practical application value for the growth of the molecular beam epitaxy, particularly the alloy requiring two V-group sources, is beneficial to ensuring the consistency of the growth conditions of scientific research and production samples, and improves the production yield.
Drawings
FIG. 1 is a plot of beam current versus different valve opening of the arsenic source furnace under good background vacuum conditions during the test of example 1.
FIG. 2 is a schematic diagram of the reconstruction of the gallium arsenide (001) substrate surface (2X 4) of example 1.
FIG. 3 is a schematic diagram of the reconstruction of the gallium arsenide (001) substrate surface c (4X 4) of example 1.
FIG. 4 is a plot of the surface reconstruction transition point temperature versus the valve opening of the arsenic source furnace for the gallium arsenide (001) sample of example 1.
FIG. 5 is a plot of the surface reconstruction transition point temperature versus the beam current of the arsenic source furnace for a sample of gallium arsenide (001) 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 beam current of an arsenic source furnace in molecular beam epitaxy, which comprises the following steps:
(1) Under the condition of good vacuum background, a beam monitor is started, the corresponding beam sizes of the arsenic source furnace under different valve openings are measured, and a valve opening-arsenic beam curve is drawn;
(2) Regulating the valve opening of the arsenic source furnace, measuring the corresponding transition point temperature when the surface reconstruction phenomenon of the gallium arsenide sample occurs, and drawing a transition point temperature-valve opening curve;
(3) Determining the arsenic beam size corresponding to the gallium arsenide sample surface transition point temperature in the experiment according to the transition point temperature-valve opening curve and the valve opening-arsenic beam curve, and drawing the transition point temperature-arsenic beam curve;
(4) For unknown arsenic beam, measuring the temperature of the transition point of the surface reconstruction of the gallium arsenide sample, and measuring the size of the arsenic beam at the moment according to the curve of the temperature of the transition point and the arsenic beam.
To further illustrate the method, the present embodiment employs a molecular beam epitaxy apparatus, and the experiment employs a gallium arsenide (001) substrate as the test sample. Firstly, under the condition of good vacuum background, measuring the arsenic beam sizes corresponding to different valve openings of the arsenic source furnace, as shown in figure 1. Then, a gallium arsenide test sample is put in, the valve opening of the arsenic source furnace is set, the temperature of the sample is reduced from high temperature to low temperature, meanwhile, the surface reconstruction characteristic of gallium arsenide (001) is observed, and when the surface reconstruction is found to be changed from (2×4) to c (4×4), the temperature of the sample at the change point is recorded, as shown in fig. 2 and 3. A transition temperature-valve opening relationship curve is established based on the sample reaching temperature at the end of transition, as shown in fig. 4. The arsenic beam size corresponding to the surface reconstruction transition temperature can be obtained from the data curves of fig. 1 and 4, as shown in fig. 5. When the beam current of arsenic needs to be calibrated later, the temperature at which the surface reconstruction of the gallium arsenide (001) sample is converted can be tested through the steps, and then the beam current of the arsenic source furnace is calibrated according to the data of fig. 5.
Claims (3)
1. A method for determining the beam size of an arsenic source furnace in molecular beam epitaxy, comprising the following steps:
(1) Under the condition of good vacuum background, a beam monitor is started, the corresponding beam sizes of the arsenic source furnace under different valve openings are measured, and a valve opening-arsenic beam curve is drawn;
(2) Regulating the valve opening of the arsenic source furnace, measuring the corresponding transition point temperature when the surface reconstruction phenomenon of the gallium arsenide sample occurs, and drawing a transition point temperature-valve opening curve;
(3) Determining the arsenic beam size corresponding to the gallium arsenide sample surface transition point temperature in the experiment according to the transition point temperature-valve opening curve and the valve opening-arsenic beam curve, and drawing the transition point temperature-arsenic beam curve;
(4) For unknown arsenic beam, measuring the temperature of the transition point of the surface reconstruction of the gallium arsenide sample, and measuring the size of the arsenic beam at the moment according to the curve of the temperature of the transition point and the arsenic beam.
2. The method according to claim 1, characterized in that: and (3) determining the surface transition point temperature of the gallium arsenide sample by using high-energy electron diffraction in the step (2).
3. The method according to claim 1, characterized in that: the reconstruction phenomenon in the step (2) refers to the transformation of the surface reconstruction of the gallium arsenide sample from (2×4) to c (4×4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311337911.9A CN117518226A (en) | 2023-10-17 | 2023-10-17 | Method for marking arsenic source furnace beam current size in molecular beam epitaxy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311337911.9A CN117518226A (en) | 2023-10-17 | 2023-10-17 | Method for marking arsenic source furnace beam current size in molecular beam epitaxy |
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| Publication Number | Publication Date |
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| CN117518226A true CN117518226A (en) | 2024-02-06 |
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| CN202311337911.9A Pending CN117518226A (en) | 2023-10-17 | 2023-10-17 | Method for marking arsenic source furnace beam current size in molecular beam epitaxy |
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| CN (1) | CN117518226A (en) |
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2023
- 2023-10-17 CN CN202311337911.9A patent/CN117518226A/en active Pending
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